Silk-Based Moisturizer Compositions and Methods Thereof

ABSTRACT

In an embodiment, a moisturizing composition includes a silk solution, wherein the silk solution comprises about 1% to about 10% (w/v) of pure silk fibroin-based protein fragments that are substantially devoid of sericin; hyaluronic acid; an oil or butter; and a pH adjusting agent.

CROSS-REFERENCE TO RELATED APPLICATIONS

This application is an international application claiming the benefit ofU.S. Provisional Application No. 62/154,581, filed on Apr. 29, 2015, theentirety of which is incorporated herein by reference.

FIELD OF THE INVENTION

The present invention relates generally to compositions that includesilk protein and more particularly, but not exclusively, to moisturizingcompositions that include a silk solution that may comprise about 0.05%to about 10% (w/v) of pure silk fibroin-based protein fragments that aresubstantially devoid of sericin.

BACKGROUND OF THE INVENTION

Silk is a natural polymer produced by a variety of insects and spiders.Silk comprises a filament core protein, silk fibroin, and a glue-likecoating consisting of a non-filamentous protein, sericin. Silk has beenhistorically studied for use in the medical field. Silk has been welldescribed in its natural fibrous form and is being studied further forpotentially useful secondary forms such as silk gels, sponges, serums,films, powders and composites. Many of these secondary forms can only becreated after processing the silk fibers into an aqueous silk solution.

Silk solutions have been generated using a variety of methods with thefinal solutions having a range of characteristics and varying levels ofpurity. Silk solutions have not only been used in medical applications,but have also expanded to other areas such as cosmetics and electronics.

BRIEF SUMMARY OF THE INVENTION

Silk protein fragment compositions and moisturizers manufacturedtherefrom are disclosed herein. In an embodiment, an article of thepresent disclosure is a silk moisturizer comprising silk proteinfragment compositions. In an embodiment, a silk moisturizer of thepresent disclosure can be used to address fine lines and wrinkles of theskin, for example fine lines and wrinkles around the mouth and nose. Inan embodiment, a silk moisturizer of the present disclosure can be usedto address dark spots on the skin. In an embodiment, a silk moisturizerof the present disclosure is used for reducing puffy eyes. In anembodiment, a silk moisturizer of the present disclosure is used forreducing dark circles around the eyes. In an embodiment, a silk gel ofthe present disclosure can be used as a firming eye moisturizer. In anembodiment, a silk moisturizer of the present disclosure can replenishmoisture and increase cell renewal while restoring radiance. In anembodiment, a silk moisturizer of the present disclosure can be used asa hydrating moisturizer to restore hydration to the skin. In anembodiment, a silk moisturizer of the present disclosure can be used totreat redness, acne and hyperpigmentation of the skin. In an embodiment,an article of the present disclosure is a silk sunscreen moisturizer.

According to aspects illustrated herein, there is disclosed amoisturizing composition including a silk solution, hyaluronic acid, anoil or butter, and a pH adjusting agent. In some embodiments the silksolution may include about 1% to about 10% (w/v) of pure silkfibroin-based protein fragments that are substantially devoid ofsericin. In some embodiments the pure silk fibroin-based proteinfragments have an average weight molecular weight ranging from about 6kDa to about 16 kDa, from about 17 kDa to about 38 kDa, or from about 39kDa to about 80 kDa. In some embodiments the pure silk fibroin-basedprotein fragments have a polydispersity of between about 1.5 and about3.0. In some embodiments the oil or butter is jojoba oil, rosehip oil,glycerin, coconut oil, lemongrass oil, or shea butter. In someembodiments a moisturizing compositions may further include a second oilor butter. In some embodiments the second oil or butter is jojoba oil,rosehip oil, glycerin, coconut oil, lemongrass oil, or shea butter. Insome embodiments the first oil or butter is present in an amount ofabout 0.1% to about 25% (v/v) of the moisturizing composition. In someembodiments the second oil or butter is present in an amount of about0.1% to about 25% (v/v) of the moisturizing composition. In someembodiments the pH adjusting agent is NaOH. In other embodiments the pHadjusting agent is HCl. In still other embodiments the pH adjustingagent includes a second pH adjusting agent. In some embodiments one ofthe first pH adjusting agent and the second pH adjusting agent is NaOHand the other of the first pH adjusting agent and the second pHadjusting agent is HCl. In some embodiments a moisturizing compositionfurther includes an additive. Example additives include vitamin E, aspenbark, sodium anisate, oat flour, titanium dioxide, and combinationsthereof. In some embodiments the additive is a combination of vitamin E,aspen bark, and sodium anisate. In some embodiments a moisturizingcomposition further comprises water.

According to aspects illustrated herein, there is disclosed a method forpreparing a moisturizer composition of pure silk fibroin-based proteinfragments including: introducing water into a vessel; adding hyaluronicacid powder is added to the water; mixing the hyaluronic acid and waterto form a solution; adding a solution of pure silk fibroin based proteinfragments to the hyaluronic acid solution, wherein the pure silk fibroinbased protein fragments are substantially devoid of sericin; mixing thehyaluronic acid and pure silk fibroin based protein fragments;introducing one or more oils and/or butters and a pH adjusting agent tothe hyaluronic acid/pure silk fibroin protein solution; mixing until awhite, lotion-like homogeneous mixture is formed. In some embodiments amethod further includes adding an additive to the hyaluronic acid/puresilk fibroin protein solution, and/or adding an additive to the white,white, lotion-like homogenous mixture and mixing. In some embodimentsthe oil and/or butter is jojoba oil, rosehip oil, glycerin, coconut oil,lemongrass oil, shea butter, or a combination thereof. In someembodiments the pure silk fibroin-based protein fragments have anaverage weight molecular weight ranging from about 6 kDa to about 16kDa, from about 17 kDa to about 38 kDa, or from about 39 kDa to about 80kDa. In some embodiments the pure silk fibroin-based protein fragmentshave a polydispersity of between about 1.5 and about 3.0.

In some embodiments the silk solution (or pure silk fibroin basedprotein fragments) is substantially homogenous, wherein the silksolution includes between 0 ppm and about 500 ppm of inorganicresiduals, and wherein the silk solution includes between 0 ppm andabout 500 ppm of organic residuals. In an embodiment, the silk solutionhas between about 10 ppm and about 300 ppm of lithium bromide residualsand between about 10 ppm and about 100 ppm of sodium carbonateresiduals. In an embodiment, the lithium bromide residuals aremeasurable using a high-performance liquid chromatography lithiumbromide assay, and the sodium carbonate residuals are measurable using ahigh-performance liquid chromatography sodium carbonate assay. In anembodiment, the pure silk fibroin-based protein fragments are in theform of a solution. In an embodiment, the silk solution compositionincludes from about 0.1 wt % to about 30 wt % pure silk fibroin-basedprotein fragments. In other embodiments, the silk solution compositionincludes from about 0.1 wt % to about 20 wt %, 1% to about 15%, about 2%to about 10%, about 5%, about 6%, or about 7% pure silk fibroin-basedprotein fragments. The pure silk fibroin-based protein fragments may bestable in the solution for at least 30 days. In an embodiment, the term“stable” refers to the absence of spontaneous or gradual gelation, withno visible change in the color or turbidity of the solution. In anembodiment, the term “stable” refers to no aggregation of fragments andtherefore no increase in molecular weight over time. In an embodiment,the silk solution composition is in the form of an aqueous solution. Inan embodiment, the silk solution composition is in the form of anorganic solution. The silk solution composition may be provided in asealed container. In some embodiments, the composition further includesone or more molecules selected from the group consisting of therapeuticagents, growth factors, antioxidants, proteins, vitamins, carbohydrates,polymers, nucleic acids, salts, acids, bases, biomolecules, glycosaminoglycans, polysaccharides, extracellular matrix molecules, metals, metalion, metal oxide, synthetic molecules, polyanhydrides, ceils, fattyacids, fatty alcohols, emollients, humectants, acid salts, emulsifiers,chelating agents fragrance, minerals, plants, plant extracts,preservatives, proteoglycans, essential oils, peptides, alcohols,tinting agents, titanium dioxide, zinc oxide, oat flour, and chemical UVfilters. In an embodiment, the added molecule or molecules are stable(i.e., retain activity over time) within the composition and can bereleased at a desired rate. In an embodiment, the one or more moleculesis vitamin C, Vitamin B, Vitamin A, or a derivative thereof. In anembodiment, the composition further includes an alpha hydroxy acidselected from the group consisting of glycolic acid, lactic acid,tartaric acid and citric acid. In an embodiment, the composition furtherincludes hyaluronic acid or its salt form at a concentration of about0.5% to about 10.0%. In an embodiment, the composition further includesat least one of zinc oxide or titanium dioxide. In an embodiment, thepure silk fibroin-based protein fragments in the composition arehypoallergenic. In an embodiment, the pure silk fibroin-based proteinfragments are biocompatible, non-sensitizing, and non-immunogenic. In anembodiment, the pure silk fibroin-based protein fragments arebioresorbable or biodegradable following implantation or application. Inan embodiment, the pure silk fibroin-based protein fragments arehypoallergenic.

According to aspects illustrated herein, there is disclosed a silksolution composition that includes pure silk fibroin-based proteinfragments that are substantially devoid of sericin, wherein the silksolution composition has an average weight average molecular weightranging from about 39 kDa to about 80 kDa, wherein the silk solutioncomposition has a polydispersity of between about 1.5 and about 3.0,wherein the silk solution composition is substantially homogenous,wherein the silk solution composition includes between 0 ppm and about500 ppm of inorganic residuals, and wherein the silk solutioncomposition includes between 0 ppm and about 500 ppm of organicresiduals, in an embodiment, the pure silk fibroin-based proteinfragments have between about 10 ppm and about 300 ppm of lithium bromideresiduals and between about 10 ppm and about 100 ppm of sodium carbonateresiduals. In an embodiment, the lithium bromide residuals aremeasurable using a high-performance liquid chromatography lithiumbromide assay, and the sodium carbonate residuals are measurable using ahigh-performance liquid chromatography sodium carbonate assay. In anembodiment, the silk solution composition is in the form of a solution.In an embodiment, the silk solution composition includes from about 0.1wt % to about 30.0 wt % pure silk fibroin-based protein fragments. Inother embodiments, the silk solution composition includes from about 0.1wt % to about 20 wt %, 1% to about 15%, about 2% to about 10%, about 5%,about 6%, or about 7% pure silk fibroin-based protein fragments. Thepure silk fibroin-based protein fragments are stable in the solution forat least 30 days. In an embodiment, the term “stable” refers to theabsence of spontaneous or gradual gelation, with no visible change inthe color or turbidity of the solution. In an embodiment, the term“stable” refers to no aggregation of fragments and therefore no increasein molecular weight over time. In an embodiment, the composition is inthe form of an aqueous solution. In an embodiment, the composition is inthe form of an organic solution. The composition may be provided in asealed container. In some embodiments, the composition further includesone or more molecules selected from the group consisting of therapeuticagents, growth factors, antioxidants, proteins, vitamins, carbohydrates,polymers, nucleic acids, salts, acids, bases, biomolecules, glycosaminoglycans, polysaccharides, extracellular matrix molecules, metals, metalion, metal oxide, synthetic molecules, polyanhydrides, cells, fattyacids, fragrance, minerals, plants, plant extracts, preservatives andessential oils. In an embodiment, the added molecule or molecules arestable (i.e., retain activity over time) within the composition and canbe released at a desired rate. In an embodiment, the one or moremolecules is vitamin C, Vitamin B, Vitamin A, or a derivative thereof.In an embodiment, the composition further includes an alpha hydroxy acidselected from the group consisting of glycolic acid, lactic acid,tartaric acid and citric acid. In an embodiment, the composition furtherincludes hyaluronic acid or its salt form at a concentration of about0.5% to about 10.0%. In an embodiment, the composition further includesat least one of zinc oxide or titanium dioxide. In an embodiment, thepure silk fibroin-based protein fragments in the composition arehypoallergenic. In an embodiment, the pure silk fibroin-based proteinfragments are biocompatible, non-sensitizing, and non-immunogenic. In anembodiment, the pure silk fibroin-based protein fragments arebioresorbable or biodegradable following implantation or application.

According to aspects illustrated herein, there is disclosed amoisturizing composition that includes pure silk fibroin-based proteinfragments substantially devoid of sericin and comprising: an averageweight average molecular weight ranging from about 17 kDa to about 38kDa; and a polydispersity of between about 1.5 and about 3.0, whereinthe moisturizing composition has a water content ranging from about 2.0wt. % to about 20.0 wt. %, wherein the moisturizing composition includesbetween about 0 ppm and about 500 ppm of inorganic residuals, whereinthe moisturizing composition includes between about 0 ppm and about 500ppm of organic residuals. In an embodiment, the moisturizing compositionincludes between about 1.0% and about 50.0% crystalline protein domainsand being soluble when submersed in water at room temperature. In anembodiment, the moisturizing composition includes from about 1 wt. % toabout 30 wt. % of pure silk fibroin-based protein fragments. In otherembodiments, the silk solution composition includes from about 0.1 wt %to about 20 wt %, 1% to about 15%, about 2% to about 10%, about 5%,about 6%, or about 7% pure silk fibroin-based protein fragments.

In an embodiment, the moisturizing composition has a pH from about 1.0to about 8.0. In an embodiment, the moisturizing composition furtherincludes one or more molecules selected from the group consisting oftherapeutic agents, growth factors, antioxidants, proteins,carbohydrates, polymers, nucleic acids, salts, acids, bases,biomolecules, glycosamino glycans, polysaccharides, extracellular matrixmolecules, metals, metal ion, metal oxide, synthetic molecules,polyanhydrides, cells, fatty acids, fragrance, minerals, plants, plantextracts, preservatives and essential oils. In an embodiment, themoisturizing composition further includes an alpha hydroxy acid selectedfrom the group consisting of glycolic acid, lactic acid, tartaric acidand citric acid. In an embodiment, the moisturizing composition furtherincludes hyaluronic acid or its salt form at a concentration rangingfrom about 0.5 wt. % to about 10.0 wt. %. In an embodiment, themoisturizing composition further includes at least one of zinc oxide ortitanium dioxide. In an embodiment, the moisturizing composition furtherincludes an additive selected from vitamin E, aspen bark, sodiumanisate, oat flour, titanium dioxide, honeysuckle blend, or combinationsthereof. In an embodiment, the moisturizing composition is packaged inan airtight container. In an embodiment, the moisturizing composition issufficiently designed for topical application. In an embodiment, thetopical application is for cosmetic use. In an embodiment, the topicalapplication is for wound dressing.

In an embodiment, a method of reducing fine lines and wrinkles includesapplying a moisturizing composition of the present disclosure daily tohuman skin for a period of at least one week and observing a reductionin fine lines and wrinkles on the human skin. In an embodiment, a methodof smoothing and rejuvenating human skin includes applying amoisturizing composition of the present disclosure daily to human skinfor a period of at least one week and observing an improvement in skintexture. In an embodiment, a method of moisturizing human skin includesapplying daily a moisturizing composition of the present disclosure tohuman skin for a period of at least one week and observing animprovement in skin hydration. In an embodiment, a method ofmoisturizing human skin includes applying twice daily a moisturizingcomposition of the present disclosure to human skin for a period of atleast one week and observing an improvement in skin hydration.

According to aspects illustrated herein, there is disclosed a method forpreparing an aqueous solution of pure silk fibroin-based proteinfragments having an average weight average molecular weight ranging fromabout 6 kDa to about 16 kDa, the method including the steps of:degumming a silk source by adding the silk source to a boiling (100° C.)aqueous solution of sodium carbonate for a treatment time of betweenabout 30 minutes to about 60 minutes; removing sericin from the solutionto produce a silk fibroin extract comprising non-detectable levels ofsericin; draining the solution from the silk fibroin extract; dissolvingthe silk fibroin extract in a solution of lithium bromide having astarting temperature upon placement of the silk fibroin extract in thelithium bromide solution that ranges from about 60° C. to about 140° C.;maintaining the solution of silk fibroin-lithium bromide in an ovenhaving a temperature of about 140° C. for a period of at least 1 hour;removing the lithium bromide from the silk fibroin extract; andproducing an aqueous solution of silk protein fragments, the aqueoussolution comprising: fragments having an average weight averagemolecular weight ranging from about 6 kDa to about 16 kDa, and whereinthe aqueous solution of pure silk fibroin-based protein fragmentscomprises a polydispersity of between about 1.5 and about 3.0. In anembodiment, the method includes the step of drying the silk fibroinextract prior to the dissolving step. In an embodiment, the amount oflithium bromide residuals in the aqueous solution can be measured usinga high-performance liquid chromatography lithium bromide assay. In anembodiment, the amount of sodium carbonate residuals in the aqueoussolution can be measured using a high-performance liquid chromatographysodium carbonate assay. In an embodiment, the method includes the stepof adding a therapeutic agent to the aqueous solution of pure silkfibroin-based protein fragments. In an embodiment, the method includesthe step of adding a molecule selected from one of an antioxidant or anenzyme to the aqueous solution of pure silk fibroin-based proteinfragments. In an embodiment, the method includes the step of adding avitamin to the aqueous solution of pure silk fibroin-based proteinfragments. In an embodiment, the vitamin is selected from one of vitaminC, vitamin B, vitamin A, or a derivative thereof. In an embodiment, themethod further includes the step of adding an alpha hydroxy acid to theaqueous solution of pure silk fibroin-based protein fragments. In anembodiment, the alpha hydroxy acid is selected from the group consistingof glycolic acid, lactic acid, tartaric acid and citric acid. In anembodiment, the method further includes the step of adding hyaluronicacid at a concentration of about 0.5% to about 10.0% to the aqueoussolution of pure silk fibroin-based protein fragments. In an embodiment,the method further includes the step of adding at least one of zincoxide or titanium dioxide to the aqueous solution of pure silkfibroin-based protein fragments. In an embodiment, the method furtherincludes the step of lyophilizing the aqueous solution of pure silkfibroin-based protein fragments. In an embodiment, a cosmetic film isfabricated from the aqueous solution of silk protein fragments. In anembodiment, a cosmetic gel is fabricated from the aqueous solution ofsilk protein fragments.

According to aspects illustrated herein, there is disclosed a method forpreparing an aqueous solution of pure silk fibroin-based proteinfragments having an average weight average molecular weight ranging fromabout 17 kDa to about 38 kDa, the method including the steps of: addinga silk source to a boiling (100° C.) aqueous solution of sodiumcarbonate for a treatment time of between about 30 minutes to about 60minutes so as to result in degumming; removing sericin from the solutionto produce a silk fibroin extract comprising non-detectable levels ofsericin; draining the solution from the silk fibroin extract; dissolvingthe silk fibroin extract in a solution of lithium bromide having astarting temperature upon placement of the silk fibroin extract in thelithium bromide solution that ranges from about 80° C. to about 140° C.;maintaining the solution of silk fibroin-lithium bromide in a dry ovenhaving a temperature in the range between about 60° C. to about 100° C.for a period of at least 1 hour; removing the lithium bromide from thesilk fibroin extract; and producing an aqueous solution of pure silkfibroin-based protein fragments, wherein the aqueous solution of puresilk fibroin-based protein fragments comprises lithium bromide residualsof between about 10 ppm and about 300 ppm, wherein the aqueous solutionof silk protein fragments comprises sodium carbonate residuals ofbetween about 10 ppm and about 100 ppm, wherein the aqueous solution ofpure silk fibroin-based protein fragments comprises fragments having anaverage weight average molecular weight ranging from about 17 kDa toabout 38 kDa, and wherein the aqueous solution of pure silkfibroin-based protein fragments comprises a polydispersity of betweenabout 1.5 and about 3.0. In an embodiment, the method includes the stepof drying the silk fibroin extract prior to the dissolving step. In anembodiment, the amount of lithium bromide residuals in the aqueoussolution can be measured using a high-performance liquid chromatographylithium bromide assay. In an embodiment, the amount of sodium carbonateresiduals in the aqueous solution can be measured using ahigh-performance liquid chromatography sodium carbonate assay. In anembodiment, the method includes the step of adding a therapeutic agentto the aqueous solution of pure silk fibroin-based protein fragments. Inan embodiment, the method includes the step of adding a moleculeselected from one of an antioxidant or an enzyme to the aqueous solutionof pure silk fibroin-based protein fragments. In an embodiment, themethod includes the step of adding a vitamin to the aqueous solution ofpure silk fibroin-based protein fragments. In an embodiment, the vitaminis selected from one of vitamin C, vitamin B, vitamin A, or a derivativethereof. In an embodiment, the method further includes the step ofadding an alpha hydroxy acid to the aqueous solution of pure silkfibroin-based protein fragments. In an embodiment, the alpha hydroxyacid is selected from the group consisting of glycolic acid, lacticacid, tartaric acid and citric acid. In an embodiment, the methodfurther includes the step of adding hyaluronic acid at a concentrationof about 0.5% to about 10.0% to the aqueous solution of pure silkfibroin-based protein fragments. In an embodiment, the method furtherincludes the step of adding at least one of zinc oxide or titaniumdioxide to the aqueous solution of pure silk fibroin-based proteinfragments. In an embodiment, the method further includes the step oflyophilizing the aqueous solution of pure silk fibroin-based proteinfragments. In an embodiment, a moisturizing composition is fabricatedfrom the aqueous solution of silk protein fragments.

According to aspects illustrated herein, there is disclosed a method forpreparing an aqueous solution of pure silk fibroin-based proteinfragments having an average weight average molecular weight ranging fromabout 39 kDa to about 80 kDa, the method including the steps of: addinga silk source to a boiling (100° C.) aqueous solution of sodiumcarbonate for a treatment time of about 30 minutes so as to result indegumming; removing sericin from the solution to produce a silk fibroinextract comprising non-detectable levels of sericin; draining thesolution from the silk fibroin extract; dissolving the silk fibroinextract in a solution of lithium bromide having a starting temperatureupon placement of the silk fibroin extract in the lithium bromidesolution that ranges from about 80° C. to about 140° C.; maintaining thesolution of silk fibroin-lithium bromide in a dry oven having atemperature in the range between about 60° C. to about 100° C. for aperiod of at least 1 hour; removing the lithium bromide from the silkfibroin extract; and producing an aqueous solution of pure silkfibroin-based protein fragments, wherein the aqueous solution of puresilk fibroin-based protein fragments comprises lithium bromide residualsof between about 10 ppm and about 300 ppm, sodium carbonate residuals ofbetween about 10 ppm and about 100 ppm, fragments having an averageweight average molecular weight ranging from about 40 kDa to about 65kDa, and wherein the aqueous solution of pure silk fibroin-based proteinfragments comprises a polydispersity of between about 1.5 and about 3.0.In an embodiment, the method includes the step of drying the silkfibroin extract prior to the dissolving step, in an embodiment, theamount of lithium bromide residuals in the aqueous solution can bemeasured using a high-performance liquid chromatography lithium bromideassay. In an embodiment, the amount of sodium carbonate residuals in theaqueous solution can be measured using a high-performance liquidchromatography sodium carbonate assay. In an embodiment, the methodincludes the step of adding a therapeutic agent to the aqueous solutionof pure silk fibroin-based protein fragments. In an embodiment, themethod includes the step of adding a molecule selected from one of anantioxidant or an enzyme to the aqueous solution of pure silkfibroin-based protein fragments. In an embodiment, the method includesthe step of adding a vitamin to the aqueous solution of pure silkfibroin-based protein fragments. In an embodiment, the vitamin isselected from one of vitamin C, vitamin B, vitamin A, or a derivativethereof, in an embodiment, the method further includes the step ofadding an alpha hydroxy acid to the aqueous solution of pure silkfibroin-based protein fragments. In an embodiment, the alpha hydroxyacid is selected from the group consisting of glycolic acid, lacticacid, tartaric acid and citric acid. In an embodiment, the methodfurther includes the step of adding hyaluronic acid at a concentrationof about 0.5% to about 10.0% to the aqueous solution of pure silkfibroin-based protein fragments. In an embodiment, the method furtherincludes the step of adding at least one of zinc oxide or titaniumdioxide to the aqueous solution of pure silk fibroin-based proteinfragments. In an embodiment, the method further includes the step oflyophilizing the aqueous solution of pure silk fibroin-based proteinfragments. In an embodiment, a moisturizing composition is fabricatedfrom the aqueous solution of silk protein fragments.

According to aspects illustrated herein, moisturizing compositionsmanufactured from SPF mixture solutions of the present disclosure aredisclosed.

BRIEF DESCRIPTION OF THE DRAWINGS

The presently disclosed embodiments will be further explained withreference to the attached drawings and appendix. The drawings shown arenot necessarily to scale, with emphasis instead generally being placedupon illustrating the principles of the presently disclosed embodiments.

FIG. 1 is a flow chart showing various embodiments for producing puresilk fibroin-based protein fragments (SPFs) of the present disclosure.

FIG. 2 is a flow chart, showing various parameters that can be modifiedduring the process of producing SPFs of the present disclosure duringthe extraction and the dissolution steps.

FIG. 3 is a photograph showing dry extracted silk fibroin.

FIG. 4 is a photograph showing an embodiment of a SPF in the form of asolution of the present disclosure.

FIGS. 5A-5D are photographs showing dissolved silk in room temperaturelithium bromide (LiBr) solutions dissolved in a 60° C. oven for 4 hours(sericin extraction temperature and time were varied).

FIGS. 6A-6D are photographs showing dissolved silk in room temperatureLiBr solutions dissolved in a 60° C. oven for 6 hours (sericinextraction temperature and time were varied).

FIGS. 7A-7D are photographs showing dissolved silk in room temperatureLiBr solutions dissolved in a 60° C. oven for 8 hours (sericinextraction temperature and time were varied).

FIGS. 8A-8D are photographs showing dissolved silk in room temperatureLiBr solutions dissolved in a 60° C. oven for 12 hours (sericinextraction temperature and time were varied).

FIGS. 9A-9D are photographs showing dissolved silk in room temperatureLiBr solutions dissolved in a 60° C. oven for 24 hours (sericinextraction temperature and time were varied).

FIGS. 10A-10D are photographs showing dissolved silk in room temperatureLiBr solutions dissolved in a 60° C. oven for 168/192 hours (sericinextraction temperature and time were varied).

FIGS. 11A-11C are photographs showing dissolved silk in room temperatureLiBr solutions dissolved in 60° C. oven for 1, 4, and 6 hours, wheresericin extraction was completed at 100° C. for 60 min.

FIGS. 12A-12D are photographs showing dissolved silk in 60° C. LiBrsolutions dissolved in a 60° C. oven for 1 hour (sericin extractiontemperature and time were varied).

FIGS. 13A-13D are photographs showing dissolved silk in 60° C. LiBrsolutions dissolved in a 60° C. oven for 4 hours (sericin extractiontemperature and time were varied).

FIGS. 14A-14D are photographs showing dissolved silk in 60° C. LiBrsolutions dissolved in a 60° C. oven for 6 hours (sericin extractiontemperature and time were varied).

FIGS. 15A-15D are photographs showing dissolved silk in 80° C. LiBrsolutions dissolved in a 60° C. oven for 1 hour (sericin extractiontemperature and time were varied).

FIGS. 16A-16D are photographs showing dissolved silk in 80° C. LiBrsolutions dissolved in a 60° C. oven for 4 hours (sericin extractiontemperature and time were varied).

FIGS. 17A-17D are photographs showing dissolved silk in 80° C. LiBrsolutions dissolved in a 60° C. oven for 6 hours (sericin extractiontemperature and time were varied).

FIGS. 18A-18D are photographs showing dissolved silk in 100° C. LiBrsolutions dissolved in a 60° C. oven for 1 hour (sericin extractiontemperature and time were varied).

FIGS. 19A-19D are photographs showing dissolved silk in 100° C. LiBrsolutions dissolved in a 60° C. oven for 4 hours (sericin extractiontemperature and time were varied).

FIGS. 20A-20D are photographs showing dissolved silk in 100° C. LiBrsolutions dissolved in a 60° C. oven for 6 hours (sericin extractiontemperature and time were varied).

FIGS. 21A-21D are photographs showing dissolved silk in 140° C. (boilingpoint for LiBr) LiBr solutions dissolved in a 60° C. oven for 1 hour(sericin extraction temperature and time were varied time).

FIGS. 22A-22D are photographs showing dissolved silk in 140° C. (boilingpoint for LiBr) LiBr solutions dissolved in a 60° C. oven for 4 hours(sericin extraction temperature and time were varied).

FIGS. 23A-23D are photographs showing dissolved silk in 140° C. (boilingpoint for LiBr) LiBr solutions dissolved in a 60° C. oven for 6 hours(sericin extraction temperature and time were varied).

FIGS. 24A-24D are photographs showing dissolved silk in 80° C. LiBrsolutions dissolved in a 80° C. oven for 1 hour (sericin extractiontemperature and time were varied).

FIGS. 25A-25D are photographs showing dissolved silk in 80° C. LiBrsolutions dissolved in a 80° C. oven for 4 hours (sericin extractiontemperature and time were varied).

FIGS. 26A-26D are photographs showing dissolved silk in 80° C. LiBrsolutions dissolved in a 80° C. oven for 6 hours (sericin extractiontemperature and time were varied).

FIGS. 27A-27D are photographs showing dissolved silk in 100° C. LiBrsolutions dissolved in a 100° C. oven for 1 hour (sericin extractiontemperature and time were varied).

FIGS. 28A-28D are photographs showing dissolved silk in 100° C. LiBrsolutions dissolved in a 100° C. oven for 4 hours (sericin extractiontemperature and time were varied).

FIGS. 29A-29D are photographs showing dissolved silk in 100° C. LiBrsolutions dissolved in a 100° C. oven for 6 hours (sericin extractiontemperature and time were varied).

FIGS. 30A-30D are photographs showing dissolved silk in 140° C. (boilingpoint for LiBr) LiBr solutions dissolved in a 120° C. oven for 1 hour(sericin extraction temperature and time were varied).

FIGS. 31A-31D are photographs showing dissolved silk in 140° C. (boilingpoint for LiBr) LiBr solutions dissolved in a 120° C. oven for 4 hours(sericin extraction temperature and time were varied).

FIG. 32A-32D are photographs showing dissolved silk in 140° C. (boilingpoint for LiBr) LiBr solutions dissolved in a 120° C. oven for 6 hours(sericin extraction temperature and time were varied).

FIG. 33 is a flow chart showing an embodiment for producing a silk filmof the present disclosure from a silk solution of the presentdisclosure.

FIG. 34 summarizes an embodiment of parameters for a silk film dryingstudy of the present disclosure.

FIG. 35 is a graph showing silk film drying times (under various airflow and temperature conditions).

FIGS. 36A and 36B show HPLC chromatograms from samples comprisingvitamin C.

FIG. 36A shows peaks from (1) a chemically stabilized sample of vitaminC at ambient conditions and (2) a sample of vitamin C taken after 1 hourat ambient conditions without chemical stabilization to preventoxidation, where degradation products are visible. FIG. 36B shows peaksfrom two different embodiments of silk films of the present disclosurethat were aged for at least 30 days at room temperature. No degradationproducts were visible.

FIGS. 37A-37D are photographs showing silk protein fragment-films of thepresent disclosure dried at room temperature for 48 hours with open airflow.

FIGS. 38A-38D are photographs showing silk protein fragment-films of thepresent disclosure dried at 40° C. in a convection oven for 8 hours withopen air flow.

FIGS. 39A-39D are photographs showing silk protein fragment-films of thepresent disclosure dried at 40° C. in a convection oven for 48 hourswith open air flow.

FIGS. 40A-40D are photographs showing silk protein fragment-films of thepresent disclosure dried at 40° C. in a convection oven for 48 hours inclosed dish.

FIGS. 41A-41D are photographs showing silk protein fragment-films of thepresent disclosure dried at 54° C. in a convection oven for 8 hours inopen dish.

FIGS. 42A-42D are photographs showing silk protein fragment-films of thepresent disclosure dried at 54° C. in a convection oven for 48 hours inopen dish.

FIGS. 43A-43D are photographs showing silk protein fragment-films of thepresent disclosure dried at 54° C. in a film dryer for 8 hours in opendish.

FIGS. 44A-44D are photographs showing silk protein fragment-films of thepresent disclosure dried at 54° C. in a film dryer for 48 hours in opendish.

FIGS. 45A-45D are photographs showing silk protein fragment-films of thepresent disclosure dried at room temperature in a convection oven for 48hours in open dish.

FIGS. 46A-46D are photographs showing the dissolution, in water, of theformed silk protein fragment-films of the present disclosure dried atroom temperature for 48 hours with open air flow.

FIGS. 47A-47D are photographs showing the dissolution, in water, of theformed silk protein fragment-films of the present disclosure dried at40° C. in a convection oven for 8 hours with open air flow.

FIGS. 48A-48D are photographs showing the dissolution, in water, of theformed silk protein fragment-films of the present disclosure dried at40° C. in a convection oven for 48 hours with open air flow.

FIGS. 49A-49D are photographs showing the dissolution, in water, of theformed silk protein fragment-films of the present disclosure dried at40° C. in a convection oven for 48 hours in closed dish.

FIGS. 50A-50D are photographs showing the dissolution, in water, of theformed silk protein fragment-films of the present disclosure dried at54° C. in a convection oven for 8 hours in open dish.

FIGS. 51A-51D are photographs showing the dissolution, in water, of theformed silk protein fragment-films of the present disclosure dried at54° C. in a convection oven for 48 hours in open dish.

FIGS. 52A-52D are photographs showing the dissolution, in water, of theformed silk protein fragment-films of the present disclosure dried at54° C. in a film dryer for 8 hours in open dish.

FIGS. 53A-53D are photographs showing the dissolution, in water, of theformed silk protein fragment-films of the present disclosure dried at54° C. in a film dryer for 48 hours in open dish.

FIGS. 54A-54D are photographs showing the dissolution, in water, of theformed silk protein fragment-films of the present disclosure dried atroom temperature in a convection oven for 48 hours in open dish.

FIG. 55 is a table summarizing the LiBr and Sodium Carbonate Na₂CO₃)concentration in silk protein solutions of the present disclosure.

FIG. 56 is a table summarizing the Na₂CO₃ concentration in silk proteinfragment-films of the present disclosure.

FIG. 57 is a table summarizing the LiBr concentration in silk proteinfragment-films of the present disclosure.

FIG. 58 is a table summarizing the LiBr and Na₂CO₃ concentration in silkprotein solutions of the present disclosure.

FIG. 59 is a table summarizing the vitamin C concentration in silkprotein fragment-films of the present disclosure.

FIG. 60 is a table summarizing the stability of vitamin C in chemicallystabilized solutions.

FIG. 61 is a table summarizing the Molecular Weights of silk proteinsolutions of the present disclosure.

FIGS. 62A and 62B are graphs representing the effect of extractionvolume on % mass loss.

FIG. 63 is a table summarizing the Molecular Weights of silk dissolvedfrom different concentrations of LiBr and from different extraction anddissolution sizes.

FIG. 64 is a graph summarizing the effect of Extraction Time onMolecular Weight of silk processed under the conditions of 100° C.Extraction Temperature, 100° C. LiBr and 100° C. Oven Dissolution(Oven/Dissolution Time was varied).

FIG. 65 is a graph summarizing the effect of Extraction Time onMolecular Weight of silk processed under the conditions of 100° C.Extraction Temperature, boiling LiBr and 60° C. Oven Dissolution(Oven/Dissolution Time was varied).

FIG. 66 is a graph summarizing the effect of Extraction Time onMolecular Weight of silk processed under the conditions of 100° C.Extraction Temperature, 60° C. LiBr and 60° C. Oven Dissolution(Oven/Dissolution Time was varied).

FIG. 67 is a graph summarizing the effect of Extraction Time onMolecular Weight of silk processed under the conditions of 100° C.Extraction Temperature, 80° C. LiBr and 80° C. Oven Dissolution(Oven/Dissolution Time was varied).

FIG. 68 is a graph summarizing the effect of Extraction Time onMolecular Weight of silk processed under the conditions of 100° C.Extraction Temperature, 80° C. LiBr and 60° C. Oven Dissolution(Oven/Dissolution Time was varied).

FIG. 69 is a graph summarizing the effect of Extraction Time onMolecular Weight of silk processed under the conditions of 100° C.Extraction Temperature, 100° C. LiBr and 60° C. Oven Dissolution(Oven/Dissolution Time was varied).

FIG. 70 is a graph summarizing the effect of Extraction Time onMolecular Weight of silk processed under the conditions of 100° C.Extraction Temperature, 140° C. LiBr and 140° C. Oven Dissolution(Oven/Dissolution Time was varied).

FIG. 71 is a graph summarizing the effect of Extraction Temperature onMolecular Weight of silk processed under the conditions of 60 minuteExtraction Time, 100° C. LiBr and 100° C. Oven Dissolution (OvenDissolution Time was varied).

FIG. 72 is a graph summarizing the effect of LiBr Temperature onMolecular Weight of silk processed under the conditions of 60 minuteExtraction Time, 100° C. Extraction Temperature and 60° C. OvenDissolution (Oven/Dissolution Time was varied).

FIG. 73 is a graph summarizing the effect of LiBr Temperature onMolecular Weight of silk processed under the conditions of 30 minuteExtraction Time, 100° C. Extraction Temperature and 60° C. OvenDissolution (Oven/Dissolution Time was varied).

FIG. 74 is a graph summarizing the effect of Oven/DissolutionTemperature on Molecular Weight of silk processed under the conditionsof 100° C. Extraction Temperature, 30 minute Extraction Time, and 100°C. Lithium Bromide (Oven/Dissolution Time was varied).

FIG. 75 is a graph summarizing the effect of Oven/DissolutionTemperature on Molecular Weight of silk processed under the conditionsof 100° C. Extraction Temperature, 60 minute Extraction Time, and 100°C. Lithium Bromide. (Oven/Dissolution Time was varied).

FIG. 76 is a graph summarizing the effect of Oven/DissolutionTemperature on Molecular Weight of silk processed under the conditionsof 100° C. Extraction Temperature, 60 minute Extraction Time, and 140°C. Lithium Bromide (Oven/Dissolution Time was varied).

FIG. 77 is a graph summarizing the effect of Oven/DissolutionTemperature on Molecular Weight of silk processed under the conditionsof 100° C. Extraction Temperature, 30 minute Extraction Time, and 140°C. Lithium Bromide (Oven/Dissolution Time was varied).

FIG. 78 is a graph summarizing the effect of Oven/DissolutionTemperature on Molecular Weight of silk processed under the conditionsof 100° C. Extraction Temperature, 60 minute Extraction Time, and 80° C.Lithium Bromide (Oven/Dissolution Time was varied).

FIG. 79 is a graph summarizing the Molecular Weights of silk processedunder varying conditions including Extraction Time, ExtractionTemperature, Lithium Bromide (LiBr) Temperature, Oven Temperature forDissolution, Oven Time for Dissolution.

FIG. 80 is a graph summarizing the Molecular Weights of silk processedunder conditions in which Oven/Dissolution Temperature is equal to LiBrTemperature.

FIG. 81 is a graph representing the % Activity of Vitamin C in PureProC™Gel.

FIGS. 82A-82C are photographs showing the effect of film drying on filmcolor and physical integrity after storage (most dry (FIG. 82A), leastdry (FIG. 82C)).

FIGS. 83A and 83B are photographs of a laser cut silk film,

FIG. 84 is a graph summarizing the quantity of vitamin C in a daily dose(i.e., the average amount of product used to cover a 25 cm² area ofskin) of PureProC™ and competitor products over a 30 day period.

FIG. 85 is a graph summarizing the ease of use of PureProC™ collected ina user experience.

FIG. 86 is a summary of the initial benefits of PureProC™ observed byusers and support of consumer knowledge.

FIG. 87 is a graph summarizing where trial participants used PureProC™Smoothing Gel.

FIG. 88 is a summary of the benefits to the skin after using PureProC™Smoothing Gel: Lemongrass by trial participants.

FIGS. 89A-89B are tables summarizing the effect of vitamin C with orwithout a vitamin C derivative on gelation.

FIG. 90 is a table summarizing the effect of vitamin C and vitamin Cderivatives on the formation of silk films of the present disclosure.

FIGS. 91A-91B are tables summarizing the effect of vitamin C andcaffeine on the formation of silk films of the present disclosure.

FIG. 92 is a table summarizing an embodiment of a caffeine gel of thepresent disclosure.

FIG. 93 is a table summarizing embodiments of preservative gels of thepresent disclosure.

FIGS. 94A-94C are tables summarizing embodiments of cosmetic serums ofthe present disclosure with varying additives and concentrations ofcomponents suitable for protection against ultraviolet radiation (UV).

FIGS. 95A-95C are tables summarizing embodiments of high concentrationvitamin C gels of the present disclosure.

FIG. 96 is a table summarizing the results of various gels of thepresent disclosure to evaluate the possible microbial contamination inthree different states of their use (intact, in-use, ending product).

FIG. 97 is a photograph of an embodiment of a foam product of thepresent disclosure suitable for protection against UV.

FIG. 98 is a photograph of an embodiment of a viscous liquid of thepresent disclosure suitable for protection against UV.

FIG. 99 is a photograph of an embodiment of a viscous liquid of thepresent disclosure suitable for protection against UV.

FIG. 100 is a photograph an embodiment of a foam product of the presentdisclosure suitable for protection against UV.

FIGS. 101 to 107 are photographs showing the process whereby ahyaluronic acid/silk solution is mixed with jojoba oil, rosehip oil,Vitamin E and 5N NaOH to provide a homogenous mixture.

FIG. 108 is a photograph showing jars containing moisturizer of theinvention at Day 1 of a moisturizer shelf-life pilot.

FIG. 109 is a photograph showing pumps containing moisturizer of theinvention at Day 1 of the moisturizer shelf-life pilot.

FIG. 110 is a photograph showing jars containing moisturizer of theinvention at Day 20 of the moisturizer shelf-life pilot.

FIG. 111 is a photograph showing pumps containing moisturizer of theinvention at Day 20 of the moisturizer shelf-life pilot.

FIG. 112 is a table that includes a description of various exemplarymoisturizing compositions.

While the above-identified drawings set forth presently disclosedembodiments, other embodiments are also contemplated, as noted in thediscussion. This disclosure presents illustrative embodiments by way ofrepresentation and not limitation. Numerous other modifications andembodiments can be devised by those skilled in the art which fall withinthe scope and spirit of the principles of the presently disclosedembodiments.

DETAILED DESCRIPTION OF THE INVENTION Silk Fibroin-Based ProteinFragments

As used herein, the term “fibroin” includes silk worm fibroin and insector spider silk protein. In an embodiment, fibroin is obtained fromBombyx mori.

Provided herein are methods for producing pure and highly scalable silkprotein fragment (SPF) mixture solutions that may be used acrossmultiple industries for a variety of applications. The solutions aregenerated from raw pure intact silk protein material and processed inorder to remove any sericin and achieve the desired weight averagemolecular weight (MW) and polydispersity of the fragment mixture. Selectmethod parameters may be altered to achieve distinct final silk proteinfragment characteristics depending upon the intended use. The resultingfinal fragment solution is pure silk protein fragments and water withPPM to non-detectable levels of process contaminants, levels acceptablein the pharmaceutical, medical and consumer cosmetic markets. Theconcentration, size and polydispersity of silk protein fragments in thesolution may farther be altered depending upon the desired use andperformance requirements. In an embodiment, the pure silk fibroin-basedprotein fragments in the solution are substantially devoid of sericin,have an average weight average molecular weight ranging from about 6 kDato about 16 kDa, and have a polydispersity ranging from about 1.5 andabout 3.0. In an embodiment, the pure silk fibroin-based proteinfragments in the solution are substantially devoid of sericin, have anaverage weight average molecular weight ranging from about 17 kDa toabout 38 kDa, and have a polydispersity ranging from about 1.5 and about3.0. In an embodiment, the pure silk fibroin-based protein fragments inthe solution are substantially devoid of sericin, have an average weightaverage molecular weight ranging from about 39 kDa to about 80 kDa, andhave a polydispersity ranging from about 1.5 and about 3.0.

In an embodiment, a silk solution may be used to generate moisturizingcompositions of varying consistencies by varying watercontent/concentration. Depending on the silk moisturizing compositionutilized and the methods for preparing a silk moisturizing composition,various properties are achieved. The moisturizing compositions may beloaded with at least one therapeutic agent and/or at least one molecule.

As used herein, the terms “substantially sericin free” or “substantiallydevoid of sericin” refer to silk fibers in which a majority of thesericin protein has been removed. In an embodiment, silk fibroin that issubstantially devoid of sericin refers to silk fibroin having betweenabout 0.01% (w/w) and about 10.0% (w/w) sericin. In an embodiment, silkfibroin that is substantially devoid of sericin refers to silk fibroinhaving between about 0.01% (w/w) and about 9.0% (w/w) sericin. In anembodiment, silk fibroin that is substantially devoid of sericin refersto silk fibroin having between about 0.01% (w/w) and about 8.0% (w/w)sericin. In an embodiment, silk fibroin that is substantially devoid ofsericin refers to silk fibroin having between about 0.01% (w/w) andabout 7.0% (w/w) sericin. In an embodiment, silk fibroin that issubstantially devoid of sericin refers to silk fibroin having betweenabout 0.01% (w/w) and about 6.0% (w/w) sericin. In an embodiment, silkfibroin that is substantially devoid of sericin refers to silk fibroinhaving between about 0.01% (w w) and about 5.0% (w/w) sericin. In anembodiment, silk fibroin that is substantially devoid of sericin refersto silk fibroin having between about 0%) (w/w) and about 4.0%) (w/w)sericin. In an embodiment, silk fibroin that is substantially devoid ofsericin refers to silk fibroin having between about 0.05% (w/w) andabout 4.0% (w/w) sericin. In an embodiment, silk fibroin that issubstantially devoid of sericin refers to silk fibroin having betweenabout 0.1% (w/w) and about 4.0% (w/w) sericin. In an embodiment, silkfibroin that is substantially devoid of sericin refers to silk fibroinhaving between about 0.5% (w/w) and about 4.0% (w/w) sericin. In anembodiment, silk fibroin that is substantially devoid of sericin refersto silk fibroin having between about 1.0% (w/w) and about 4.0%> (w/w)sericin. In an embodiment, silk fibroin that is substantially devoid ofsericin refers to silk fibroin having between about 1.5% (w/w) and about4.0%) (w/w) sericin. In an embodiment, silk fibroin that issubstantially devoid of sericin refers to silk fibroin having betweenabout 2.0% (w/w) and about 4.0%) (w/w) sericin. In an embodiment, silkfibroin that is substantially devoid of sericin refers to silk fibroinhaving between about 2.5% (w/w) and about 4.0% (w/w) sericin. In anembodiment, silk fibroin that is substantially devoid of sericin refersto silk fibroin having a sericin content between about 0.01% (w/w) andabout 0.1% (w/w). In an embodiment, silk fibroin that is substantiallydevoid of sericin refers to silk fibroin having a sericin content belowabout 0.1% (w/w). In an embodiment, silk fibroin that is substantiallydevoid of sericin refers to silk fibroin having a sericin content belowabout 0.05% (w/w). In an embodiment, when a silk source is added to aboiling (100° C.) aqueous solution of sodium carbonate for a treatmenttime of between about 30 minutes to about 60 minutes, a degumming lossof about 26 wt. % to about 31 wt. % is obtained.

As used herein, the term “substantially homogeneous” may refer to puresilk fibroin-based protein fragments that are distributed in a normaldistribution about an identified molecular weight. As used herein, theterm “substantially homogeneous” may refer to an even distribution ofadditive, for example vitamin C, throughout a composition of the presentdisclosure.

As used herein, the term “substantially free of inorganic residuals”means that the composition exhibits residuals of 0.1% (w/w) or less. Inan embodiment, substantially free of inorganic residuals refers to acomposition that exhibits residuals of 0.05% (w/w) or less. In anembodiment, substantially free of inorganic residuals refers to acomposition that exhibits residuals of 0.01% (w/w) or less. In anembodiment, the amount of inorganic residuals is between 0 ppm(“non-detectable” or “ND”) and 1000 ppm. In an embodiment, the amount ofinorganic residuals is ND to about 500 ppm. In an embodiment, the amountof inorganic residuals is ND to about 400 ppm. In an embodiment, theamount of inorganic residuals is ND to about 300 ppm. In an embodiment,the amount of inorganic residuals is ND to about 200 ppm. In anembodiment, the amount of inorganic residuals is ND to about 100 ppm. Inan embodiment, the amount of inorganic residuals is between 10 ppm and1000 ppm.

As used herein, the term “substantially free of organic residuals” meansthat the composition exhibits residuals of 0.1% (w/w) or less, in anembodiment, substantially free of organic residuals refers to acomposition that exhibits residuals of 0.05% (w/w) or less. In anembodiment, substantially free of organic residuals refers to acomposition that exhibits residuals of 0.01% (w/w) or less. In anembodiment, the amount of organic residuals is between 0 ppm(“non-detectable” or “ND”) and 1000 ppm. In an embodiment, the amount oforganic residuals is ND to about 500 ppm. In an embodiment, the amountof organic residuals is ND to about 400 ppm. In an embodiment, theamount of organic residuals is ND to about 300 ppm. In an embodiment,the amount of organic residuals is ND to about 200 ppm. In anembodiment, the amount of organic residuals is ND to about 100 ppm. Inan embodiment, the amount of organic residuals is between 10 ppm and1000 ppm.

Compositions of the present disclosure exhibit “biocompatibility”meaning that the compositions are compatible with living tissue or aliving system by not being toxic, injurious, or physiologically reactiveand not causing immunological rejection. Such biocompatibility can beevidenced by participants topically applying compositions of the presentdisclosure on their skin for an extended period of time. In anembodiment, the extended period of time is about 3 days. In anembodiment, the extended period of time is about 7 days, in anembodiment, the extended period of time is about 14 days, in anembodiment, the extended period of time is about 21 days. In anembodiment, the extended period of time is about 30 days. In anembodiment, the extended period of time is selected from the groupconsisting of about 1 month, about 2 months, about 3 months, about 4months, about 5 months, about 6 months, about 7 months, about 8 months,about 9 months, about 10 months, about 11 months, about 12 months, andindefinitely.

Compositions of the present disclosure are “hypoallergenic” meaning thatthey are relatively unlikely to cause an allergic reaction. Suchhypoallergenicity can be evidenced by participants topically applyingcompositions of the present disclosure on their skin for an extendedperiod of time. In an embodiment, the extended period of time is about 3days. In an embodiment, the extended period of time is about 7 days. Inan embodiment, the extended period of time is about 14 days. In anembodiment, the extended period of time is about 21 days. In anembodiment, the extended period of time is about 30 days. In anembodiment, the extended period of time is selected from the groupconsisting of about 1 month, about 2 months, about 3 months, about 4months, about 5 months, about 6 months, about 7 months, about 8 months,about 9 months, about 10 months, about 11 months, about 12 months, andindefinitely.

Following are non-limiting examples of suitable ranges for variousparameters in and for preparation of the silk solutions of the presentdisclosure. The silk solutions of the present disclosure may include oneor more, but not necessarily all, of these parameters and may beprepared using various combinations of ranges of such parameters.

In an embodiment, the percent silk in the solution is less than 30%. Inan embodiment, the percent silk in the solution is less than 25%. In anembodiment, the percent silk in the solution is less than 20%. In anembodiment, the percent silk in the solution is less than 19%. In anembodiment, the percent silk in the solution is less than 18%. In anembodiment, the percent silk in the solution is less than 17%. In anembodiment, the percent silk in the solution is less than 16%. In anembodiment, the percent silk in the solution is less than 15%. In anembodiment, the percent silk in the solution is less than 14%. In anembodiment, the percent silk in the solution is less than 13%. In anembodiment, the percent silk in the solution is less than 12%. In anembodiment, the percent silk in the solution is less than 11%. In anembodiment, the percent silk in the solution is less than 10%. In anembodiment, the percent silk in the solution is less than 9%. In anembodiment, the percent silk in the solution is less than 8%. In anembodiment, the percent silk in the solution is less than 7%. In anembodiment, the percent silk in the solution is less than 6%. In anembodiment, the percent silk in the solution is less than 5%. In anembodiment, the percent silk in the solution is less than 4%. In anembodiment, the percent silk in the solution is less than 3%. In anembodiment, the percent silk in the solution is less than 2%. In anembodiment, the percent silk in the solution is less than 1%. In anembodiment, the percent silk in the solution is less than 0.9%. In anembodiment, the percent silk in the solution is less than 0.8%. In anembodiment, the percent silk in the solution is less than 0.7%. In anembodiment, the percent silk in the solution is less than 0.6%. In anembodiment, the percent silk in the solution is less than 0.5%. In anembodiment, the percent silk in the solution is less than 0.4%. In anembodiment, the percent silk in the solution is less than 0.3%. In anembodiment, the percent silk in the solution is less than 0.2%. In anembodiment, the percent silk in the solution is less than 0.1%. In anembodiment, the percent silk in the solution is greater than 0.1%. In anembodiment, the percent silk in the solution is greater than 0.2%. In anembodiment, the percent silk in the solution is greater than 0.3%. In anembodiment, the percent silk in the solution is greater than 0.4%. In anembodiment, the percent silk in the solution is greater than 0.5%. In anembodiment, the percent silk in the solution is greater than 0.6%. In anembodiment, the percent silk in the solution is greater than 0.7%. In anembodiment, the percent silk in the solution is greater than 0.8%. In anembodiment, the percent silk in the solution is greater than 0.9%. In anembodiment, the percent silk in the solution is greater than 1%. In anembodiment, the percent silk in the solution is greater than 2%. In anembodiment, the percent silk in the solution is greater than 3%. In anembodiment, the percent silk in the solution is greater than 4%. In anembodiment, the percent silk in the solution is greater than 5%. In anembodiment, the percent silk in the solution is greater than 6%. In anembodiment, the percent silk in the solution is greater than 7%. In anembodiment, the percent silk in the solution is greater than 8%. In anembodiment, the percent silk in the solution is greater than 9%. In anembodiment, the percent silk in the solution is greater than 10%. In anembodiment, the percent silk in the solution is greater than 11%. In anembodiment, the percent silk in the solution is greater than 12%. In anembodiment, the percent silk in the solution is greater than 13%. In anembodiment, the percent silk in the solution is greater than 14%. In anembodiment, the percent silk in the solution is greater than 15%. In anembodiment, the percent silk in the solution is greater than 16%. In anembodiment, the percent silk in the solution is greater than 17%. In anembodiment, the percent silk in the solution is greater than 18%. In anembodiment, the percent silk in the solution is greater than 19%. In anembodiment, the percent silk in the solution is greater than 20%. In anembodiment, the percent silk in the solution is greater than 25%. In anembodiment, the percent silk in the solution is between 0.1% and 30%. Inan embodiment, the percent silk in the solution is between 0.1% and 25%.In an embodiment, the percent silk in the solution is between 0.1% and20%. In an embodiment, the percent silk in the solution is between 0.1%and 15%. In an embodiment, the percent silk in the solution is between0.1% and 10%. In an embodiment, the percent silk in the solution isbetween 0.1% and 9%. In an embodiment, the percent silk in the solutionis between 0.1% and 8%. In an embodiment, the percent silk in thesolution is between 0.1% and 7%. In an embodiment, the percent silk inthe solution is between 0.1% and 6.5%. In an embodiment, the percentsilk in the solution is between 0.1% and 6%. In an embodiment, thepercent silk in the solution is between 0.1% and 5.5%. In an embodiment,the percent silk in the solution is between 0.1% and 5%. In anembodiment, the percent silk in the solution is between 0.1% and 4.5%.In an embodiment, the percent silk in the solution is between 0.1% and4%. In an embodiment, the percent silk in the solution is between 0.1%and 3.5%. In an embodiment, the percent silk in the solution is between0.1% and 3%. In an embodiment, the percent silk in the solution isbetween 0.1% and 2.5%. In an embodiment, the percent silk in thesolution is between 0.1% and 2.0%. In an embodiment, the percent silk inthe solution is between 0.1% and 2.4%. In an embodiment, the percentsilk in the solution is between 0.5% and 5%. In an embodiment, thepercent silk in the solution is between 0.5% and 4.5%. In an embodiment,the percent silk in the solution is between 0.5% and 4%. In anembodiment, the percent silk in the solution is between 0.5% and 3.5%.In an embodiment, the percent silk in the solution is between 0.5% and3%. In an embodiment, the percent silk in the solution is between 0.5%and 2.5%. In an embodiment, the percent silk in the solution is between1 and 4%. In an embodiment, the percent silk in the solution is between1 and 3.5%. In an embodiment, the percent silk in the solution isbetween 1 and 3%. In an embodiment, the percent silk in the solution isbetween 1 and 2.5%. In an embodiment, the percent silk in the solutionis between 1 and 2.4%. In an embodiment, the percent silk in thesolution is between 1 and 2%. In an embodiment, the percent silk in thesolution is between 20% and 30%. In an embodiment, the percent silk inthe solution is between 0.1% and 10%. In an embodiment, the percent silkin the solution is between 1% and 10%. In an embodiment, the percentsilk in the solution is between 2% and 10%. In an embodiment, thepercent silk in the solution is between 0.1% and 6%. In an embodiment,the percent silk in the solution is between 6% and 10%. In anembodiment, the percent silk in the solution is between 6% and 8%. In anembodiment, the percent silk in the solution is between 6% and 9%. In anembodiment, the percent silk in the solution is between 10% and 20%. Inan embodiment, the percent silk in the solution is between 11% and 19%.In an embodiment, the percent silk in the solution is between 12% and18%. In an embodiment, the percent silk in the solution is between 13%and 17%. In an embodiment, the percent silk in the solution is between14% and 16%. In an embodiment, the percent silk in the solution is about1%. In an embodiment, the percent silk in the solution is about 1.5%. Inan embodiment, the percent silk in the solution is about 2%. In anembodiment, the percent silk in the solution is about 2.4%. In anembodiment, the percent silk in the solution is 3%. In an embodiment,the percent silk in the solution is 3.5%. In an embodiment, the percentsilk in the solution is about 4%. In an embodiment, the percent silk inthe solution is about 4.5%. In an embodiment, the percent silk in thesolution is about 5%. In an embodiment, the percent silk in the solutionis about 5.5%. In an embodiment the percent silk in the solution isabout 6%. In an embodiment, the percent silk in the solution is about6.5%. In an embodiment, the percent silk in the solution is about 7%. Inan embodiment, the percent silk in the solution is about 7.5%. In anembodiment, the percent silk in the solution is about 8%. In anembodiment, the percent silk in the solution is about 8.5%. In anembodiment, the percent silk in the solution is about 9%. In anembodiment, the percent silk in the solution is about 9.5%. In anembodiment, the percent silk in the solution is about 10%.

In an embodiment, the percent sericin in the solution is non-detectableto 30%. In an embodiment, the percent sericin in the solution isnon-detectable to 5%. In an embodiment, the percent sericin in thesolution is 1%. In an embodiment, the percent sericin in the solution is2%. In an embodiment, the percent sericin in the solution is 3%. In anembodiment, the percent sericin in the solution is 4%. In an embodiment,the percent sericin in the solution is 5%. In an embodiment, the percentsericin in the solution is 10%. In an embodiment, the percent sericin inthe solution is 30%.

In an embodiment, the stability of the LiBr-silk fragment solution is 0to 1 year. In an embodiment, the stability of the LiBr-silk fragmentsolution is 0 to 2 years. In an embodiment, the stability of theLiBr-silk fragment solution is 0 to 3 years. In an embodiment, thestability of the LiBr-silk fragment solution is 0 to 4 years. In anembodiment, the stability of the LiBr-silk fragment solution is 0 to 5years. In an embodiment, the stability of the LiBr-silk fragmentsolution is 1 to 2 years. In an embodiment, the stability of theLiBr-silk fragment solution is 1 to 3 years. In an embodiment, thestability of the LiBr-silk fragment solution is 1 to 4 years. In anembodiment, the stability of the LiBr-silk fragment solution is 1 to 5years. In an embodiment, the stability of the LiBr-silk fragmentsolution is 2 to 3 years. In an embodiment, the stability of theLiBr-silk fragment solution is 2 to 4 years. In an embodiment, thestability of the LiBr-silk fragment solution is 2 to 5 years. In anembodiment, the stability of the LiBr-silk fragment solution is 3 to 4years. In an embodiment, the stability of the LiBr-silk fragmentsolution is 3 to 5 years. In an embodiment, the stability of theLiBr-silk fragment solution is 4 to 5 years.

In an embodiment, the stability of a composition of the presentdisclosure is 10 days to 6 months. In an embodiment, the stability of acomposition of the present disclosure is 6 months to 12 months. In anembodiment, the stability of a composition of the present disclosure is12 months to 18 months. In an embodiment, the stability of a compositionof the present disclosure is 18 months to 24 months. In an embodiment,the stability of a composition of the present disclosure is 24 months to30 months. In an embodiment, the stability of a composition of thepresent disclosure is 30 months to 36 months. In an embodiment, thestability of a composition of the present disclosure is 36 months to 48months. In an embodiment, the stability of a composition of the presentdisclosure is 48 months to 60 months.

In an embodiment, a composition of the present disclosure includes puresilk fibroin-based protein fragments having an average weight averagemolecular weight ranging from 6 kDa to 16 kDa. In an embodiment, acomposition of the present disclosure includes pure silk fibroin-basedprotein fragments having an average weight average molecular weightranging from 17 kDa to 38 kDa. In an embodiment, a composition of thepresent disclosure includes pure silk fibroin-based protein fragmentshaving an average weight average molecular weight ranging from 39 kDa to80 kDa. In an embodiment, a composition of the present disclosureincludes pure silk fibroin-based protein fragments having an averageweight average molecular weight ranging from 1 to 5 kDa. In anembodiment, a composition of the present disclosure includes pure silkfibroin-based protein fragments having an average weight averagemolecular weight ranging from 5 to 10 kDa. In an embodiment, acomposition of the present disclosure includes pure silk fibroin-basedprotein fragments having an average weight average molecular weightranging from 10 to 15 kDa. In an embodiment, a composition of thepresent disclosure includes pure silk fibroin-based protein fragmentshaving an average weight average molecular weight ranging from 15 to 20kDa. In an embodiment, a composition of the present disclosure includespure silk fibroin-based protein fragments having an average weightaverage molecular weight ranging from 20 to 25 kDa. In an embodiment, acomposition of the present disclosure includes pure silk fibroin-basedprotein fragments having an average weight average molecular weightranging from 25 to 30 kDa. In an embodiment, a composition of thepresent disclosure includes pure silk fibroin-based protein fragmentshaving an average weight average molecular weight ranging from 30 to 35kDa. In an embodiment, a composition of the present disclosure includespure silk fibroin-based protein fragments having an average weightaverage molecular weight ranging from 35 to 40 kDa. In an embodiment, acomposition of the present disclosure includes pure silk fibroin-basedprotein fragments having an average weight average molecular weightranging from 40 to 45 kDa. In an embodiment, a composition of thepresent disclosure includes pure silk fibroin-based protein fragmentshaving an average weight average molecular weight ranging from 45 to 50kDa. In an embodiment, a composition of the present disclosure includespure silk fibroin-based protein fragments having an average weightaverage molecular weight ranging from 50 to 55 kDa. In an embodiment, acomposition of the present disclosure includes pure silk fibroin-basedprotein fragments having an average weight average molecular weightranging from 55 to 60 kDa. In an embodiment, a composition of thepresent disclosure includes pure silk fibroin-based protein fragmentshaving an average weight average molecular weight ranging from 60 to 65kDa. In an embodiment, a composition of the present disclosure includespure silk fibroin-based protein fragments having an average weightaverage molecular weight ranging from 65 to 70 kDa. In an embodiment, acomposition of the present disclosure includes pure silk fibroin-basedprotein fragments having an average weight average molecular weightranging from 70 to 75 kDa. In an embodiment, a composition of thepresent disclosure includes pure silk fibroin-based protein fragmentshaving an average weight average molecular weight ranging from 75 to 80kDa. In an embodiment, a composition of the present disclosure includespure silk fibroin-based protein fragments having an average weightaverage molecular weight ranging from 80 to 85 kDa. In an embodiment, acomposition of the present disclosure includes pure silk fibroin-basedprotein fragments having an average weight average molecular weightranging from 85 to 90 kDa. In an embodiment, a composition of thepresent disclosure includes pure silk fibroin-based protein fragmentshaving an average weight average molecular weight ranging from 90 to 95kDa. In an embodiment, a composition of the present disclosure includespure silk fibroin-based protein fragments having an average weightaverage molecular weight ranging from 95 to 100 kDa. In an embodiment, acomposition of the present disclosure includes pure silk fibroin-basedprotein fragments having an average weight average molecular weightranging from 100 to 105 kDa. In an embodiment, a composition of thepresent disclosure includes pure silk fibroin-based protein fragmentshaving an average weight average molecular weight ranging from 105 to110 kDa. In an embodiment, a composition of the present disclosureincludes pure silk fibroin-based protein fragments having an averageweight average molecular weight ranging from 110 to 115 kDa. In anembodiment, a composition of the present disclosure includes pure silkfibroin-based protein fragments having an average weight averagemolecular weight ranging from 115 to 120 kDa. In an embodiment, acomposition of the present disclosure includes pure silk fibroin-basedprotein fragments having an average weight average molecular weightranging from 120 to 125 kDa. In an embodiment, a composition of thepresent disclosure includes pure silk fibroin-based protein fragmentshaving an average weight average molecular weight ranging from 125 to130 kDa. In an embodiment, a composition of the present disclosureincludes pure silk fibroin-based protein fragments having an averageweight average molecular weight ranging from 130 to 135 kDa. In anembodiment, a composition of the present disclosure includes pure silkfibroin-based protein fragments having an average weight averagemolecular weight ranging from 135 to 140 kDa. In an embodiment, acomposition of the present disclosure includes pure silk fibroin-basedprotein fragments having an average weight average molecular weightranging from 140 to 145 kDa. In an embodiment, a composition of thepresent disclosure includes pure silk fibroin-based protein fragmentshaving an average weight average molecular weight ranging from 145 to150 kDa. In an embodiment, a composition of the present disclosureincludes pure silk fibroin-based protein fragments having an averageweight average molecular weight ranging from 150 to 155 kDa. In anembodiment, a composition of the present disclosure includes pure silkfibroin-based protein fragments having an average weight averagemolecular weight ranging from 155 to 160 kDa. In an embodiment, acomposition of the present disclosure includes pure silk fibroin-basedprotein fragments having an average weight average molecular weightranging from 160 to 165 kDa. In an embodiment, a composition of thepresent disclosure includes pure silk fibroin-based protein fragmentshaving an average weight average molecular weight ranging from 165 to170 kDa. In an embodiment, a composition of the present disclosureincludes pure silk fibroin-based protein fragments having an averageweight average molecular weight ranging from 170 to 175 kDa. In anembodiment, a composition of the present disclosure includes pure silkfibroin-based protein fragments having an average weight averagemolecular weight ranging from 175 to 180 kDa. In an embodiment, acomposition of the present disclosure includes pure silk fibroin-basedprotein fragments having an average weight average molecular weightranging from 180 to 185 kDa. In an embodiment, a composition of thepresent disclosure includes pure silk fibroin-based protein fragmentshaving an average weight average molecular weight ranging from 185 to190 kDa. In an embodiment, a composition of the present disclosureincludes pure silk fibroin-based protein fragments having an averageweight average molecular weight ranging from 190 to 195 kDa. In anembodiment, a composition of the present disclosure includes pure silkfibroin-based protein fragments having an average weight averagemolecular weight ranging from 195 to 200 kDa. In an embodiment, acomposition of the present disclosure includes pure silk fibroin-basedprotein fragments having an average weight average molecular weightranging from 200 to 205 kDa. In an embodiment, a composition of thepresent disclosure includes pure silk fibroin-based protein fragmentshaving an average weight average molecular weight ranging from 205 to210 kDa. In an embodiment, a composition of the present disclosureincludes pure silk fibroin-based protein fragments having an averageweight average molecular weight ranging from 210 to 215 kDa. In anembodiment, a composition of the present disclosure includes pure silkfibroin-based protein fragments having an average weight averagemolecular weight ranging from 215 to 220 kDa. In an embodiment, acomposition of the present disclosure includes pure silk fibroin-basedprotein fragments having an average weight average molecular weightranging from 220 to 225 kDa. In an embodiment, a composition of thepresent disclosure includes pure silk fibroin-based protein fragmentshaving an average weight average molecular weight ranging from 225 to230 kDa. In an embodiment, a composition of the present disclosureincludes pure silk fibroin-based protein fragments having an averageweight average molecular weight ranging from 230 to 235 kDa. In anembodiment, a composition of the present disclosure includes pure silkfibroin-based protein fragments having an average weight averagemolecular weight ranging from 235 to 240 kDa. In an embodiment, acomposition of the present disclosure includes pure silk fibroin-basedprotein fragments having an average weight average molecular weightranging from 240 to 245 kDa. In an embodiment, a composition of thepresent disclosure includes pure silk fibroin-based protein fragmentshaving an average weight average molecular weight ranging from 245 to250 kDa. In an embodiment, a composition of the present disclosureincludes pure silk fibroin-based protein fragments having an averageweight average molecular weight ranging from 250 to 255 kDa. In anembodiment, a composition of the present disclosure includes pure silkfibroin-based protein fragments having an average weight averagemolecular weight ranging from 255 to 260 kDa. In an embodiment, acomposition of the present disclosure includes pure silk fibroin-basedprotein fragments having an average weight average molecular weightranging from 260 to 265 kDa. In an embodiment, a composition of thepresent disclosure includes pure silk fibroin-based protein fragmentshaving an average weight average molecular weight ranging from 265 to270 kDa. In an embodiment, a composition of the present disclosureincludes pure silk fibroin-based protein fragments having an averageweight average molecular weight ranging from 270 to 275 kDa. In anembodiment, a composition of the present disclosure includes pure silkfibroin-based protein fragments having an average weight averagemolecular weight ranging from 275 to 280 kDa. In an embodiment, acomposition of the present disclosure includes pure silk fibroin-basedprotein fragments having an average weight average molecular weightranging from 280 to 285 kDa. In an embodiment, a composition of thepresent disclosure includes pure silk fibroin-based protein fragmentshaving an average weight average molecular weight ranging from 285 to290 kDa. In an embodiment, a composition of the present disclosureincludes pure silk fibroin-based protein fragments having an averageweight average molecular weight ranging from 290 to 295 kDa. In anembodiment, a composition of the present disclosure includes pure silkfibroin-based protein fragments having an average weight averagemolecular weight ranging from 295 to 300 kDa. In an embodiment, acomposition of the present disclosure includes pure silk fibroin-basedprotein fragments having an average weight average molecular weightranging from 300 to 305 kDa. In an embodiment, a composition of thepresent disclosure includes pure silk fibroin-based protein fragmentshaving an average weight average molecular weight ranging from 305 to310 kDa. In an embodiment, a composition of the present disclosureincludes pure silk fibroin-based protein fragments having an averageweight average molecular weight ranging from 310 to 315 kDa. In anembodiment, a composition of the present disclosure includes pure silkfibroin-based protein fragments having an average weight averagemolecular weight ranging from 315 to 320 kDa. In an embodiment, acomposition of the present disclosure includes pure silk fibroin-basedprotein fragments having an average weight average molecular weightranging from 320 to 325 kDa. In an embodiment, a composition of thepresent disclosure includes pure silk fibroin-based protein fragmentshaving an average weight average molecular weight ranging from 325 to330 kDa. In an embodiment, a composition of the present disclosureincludes pure silk fibroin-based protein fragments having an averageweight average molecular weight ranging from 330 to 335 kDa. In anembodiment, a composition of the present disclosure includes pure silkfibroin-based protein fragments having an average weight averagemolecular weight ranging from 350 to 340 kDa. In an embodiment, acomposition of the present disclosure includes pure silk fibroin-basedprotein fragments having an average weight average molecular weightranging from 340 to 345 kDa. In an embodiment, a composition of thepresent disclosure includes pure silk fibroin-based protein fragmentshaving an average weight average molecular weight ranging from 345 to350 kDa.

In an embodiment, a composition of the present disclosure having puresilk fibroin-based protein fragments has a polydispersity ranging fromabout 1 to about 5.0, In an embodiment, a composition of the presentdisclosure having pure silk fibroin-based protein fragments has apolydispersity ranging from about 1.5 to about 3.0. In an embodiment, acomposition of the present disclosure having pure silk fibroin-basedprotein fragments has a polydispersity ranging from about 1 to about1.5. In an embodiment, a composition of the present disclosure havingpure silk fibroin-based protein fragments has a polydispersity rangingfrom about 1.5 to about 2.0. In an embodiment, a composition of thepresent disclosure having pure silk fibroin-based protein fragments hasa polydispersity ranging from about 2.0 to about 2.5. In an embodiment,a composition of the present disclosure having pure silk fibroin-basedprotein fragments, has a polydispersity ranging from about is 2.0 toabout 3.0. In an embodiment, a composition of the present disclosurehaving pure silk fibroin-based protein fragments, has a polydispersityranging from about is 2.5 to about 3.0.

In an embodiment, a composition of the present disclosure having puresilk fibroin-based protein fragments has non-detectable levels of LiBrresiduals. In an embodiment, the amount of the LiBr residuals in acomposition of the present disclosure is between 10 ppm and 1000 ppm. Inan embodiment, the amount of the LiBr residuals in a composition of thepresent disclosure is between 10 ppm and 300 ppm. In an embodiment, theamount of the LiBr residuals in a composition of the present disclosureis less than 25 ppm. In an embodiment, the amount of the Li Br residualsin a composition of the present disclosure is less than 50 ppm. In anembodiment, the amount of the LiBr residuals in a composition of thepresent disclosure is less than 75 ppm. In an embodiment, the amount ofthe LiBr residuals in a composition of the present disclosure is lessthan 100 ppm. In an embodiment, the amount of the LiBr residuals in acomposition of the present disclosure is less than 200 ppm. In anembodiment, the amount of the LiBr residuals in a composition of thepresent disclosure is less than 300 ppm. In an embodiment, the amount ofthe LiBr residuals in a composition of the present disclosure is lessthan 400 ppm. In an embodiment, the amount of the LiBr residuals in acomposition of the present disclosure is less than 500 ppm. In anembodiment, the amount of the LiBr residuals in a composition of thepresent disclosure is less than 600 ppm. In an embodiment, the amount ofthe LiBr residuals in a composition of the present disclosure is lessthan 700 ppm. In an embodiment, the amount of the LiBr residuals in acomposition of the present disclosure is less than 800 ppm. In anembodiment, the amount of the LiBr residuals in a composition of thepresent disclosure is less than 900 ppm. In an embodiment, the amount ofthe LiBr residuals in a composition of the present disclosure is lessthan 1000 ppm. In an embodiment, the amount of the LiBr residuals in acomposition of the present disclosure is non-detectable to 500 ppm. Inan embodiment, the amount of the LiBr residuals in a composition of thepresent disclosure is non-detectable to 450 ppm. In an embodiment, theamount of the LiBr residuais in a composition of the present disclosureis non-detectable to 400 ppm. In an embodiment, the amount of the LiBrresiduals in a composition of the present disclosure is non-detectableto 350 ppm. In an embodiment, the amount of the LiBr residuals in acomposition of the present disclosure is non-detectable to 300 ppm. Inan embodiment, the amount of the LiBr residuals in a composition of thepresent disclosure is non-detectable to 250 ppm. In an embodiment, theamount of the LiBr residuals in a composition of the present disclosureis non-detectable to 200 ppm. In an embodiment, the amount of the LiBrresiduals in a composition of the present disclosure is non-detectableto 150 ppm. In an embodiment, the amount of the LiBr residuals in acomposition of the present disclosure is non-detectable to 100 ppm. Inan embodiment, the amount of the LiBr residuals in a composition of thepresent disclosure is 100 ppm to 200 ppm. In an embodiment, the amountof the LiBr residuals in a composition of the present disclosure is 200ppm to 300 ppm. In an embodiment, the amount of the LiBr residuals in acomposition of the present disclosure is 300 ppm to 400 ppm. In anembodiment, the amount of the LiBr residuals in a composition of thepresent disclosure is 400 ppm to 500 ppm.

In an embodiment, a composition of the present disclosure having puresilk fibroin-based protein fragments, has non-detectable levels ofNa₂CO₃ residuals. In an embodiment, the amount of the Na₂CO₃ residualsin a composition of the present disclosure is less than 100 ppm. In anembodiment, the amount of the Na₂CO₃ residuals in a composition of thepresent disclosure is less than 200 ppm. In an embodiment, the amount ofthe Na₂CO₃ residuals in a composition of the present disclosure is lessthan 300 ppm. In an embodiment, the amount of the Na₂CO₃ residuals in acomposition of the present disclosure is less than 400 ppm. In anembodiment, the amount of the Na₂CO₃ residuals in a composition of thepresent disclosure is less than 500 ppm. In an embodiment, the amount ofthe Na₂CO₃ residuals in a composition of the present disclosure is lessthan 600 ppm. In an embodiment, the amount of the Na₂CO₃ residuals in acomposition of the present disclosure is less than 700 ppm. In anembodiment, the amount of the Na₂CO₃ residuals in a composition of thepresent disclosure is less than 800 ppm. In an embodiment, the amount ofthe Na₂CO₃ residuals in a composition of the present disclosure is lessthan 900 ppm. In an embodiment, the amount of the Na₂CO₃ residuals in acomposition of the present disclosure is less than 1000 ppm. In anembodiment, the amount of the Na₂CO₃ residuals in a composition of thepresent disclosure is non-detectable to 500 ppm. In an embodiment, theamount of the Na₂CO₃ residuals in a composition of the presentdisclosure is non-detectable to 450 ppm. In an embodiment, the amount ofthe Na₂CO₃ residuals in a composition of the present disclosure isnon-detectable to 400 ppm. In an embodiment, the amount of the Na₂CO₃residuals in a composition of the present disclosure is non-detectableto 350 ppm. In an embodiment, the amount of the Na₂CO₃ residuals in acomposition of the present disclosure is non-detectable to 300 ppm. Inan embodiment, the amount of the Na₂CO₃ residuals in a composition ofthe present disclosure is non-detectable to 250 ppm. In an embodiment,the amount of the Na₂CO₃ residuals in a composition of the presentdisclosure is non-detectable to 200 ppm. In an embodiment, the amount ofthe Na₂CO₃ residuals in a composition of the present disclosure isnon-detectable to 150 ppm. In an embodiment, the amount of the Na₂CO₃residuals in a composition of the present disclosure is non-detectableto 100 ppm. In an embodiment, the amount of the Na₂CO₃ residuals in acomposition of the present disclosure is 100 ppm to 200 ppm. In anembodiment, the amount of the Na₂CO₃ residuals in a composition of thepresent disclosure is 200 ppm to 300 ppm. In an embodiment, the amountof the Na₂CO₃ residuals in a composition of the present disclosure is300 ppm to 400 ppm. In an embodiment, the amount of the Na₂CO₃ residualsin a composition of the present disclosure is 400 ppm to 500 ppm.

In an embodiment, the water solubility of pure silk fibroin-basedprotein fragments of the present disclosure is 50 to 100%. In anembodiment, the water solubility of pure silk fibroin-based proteinfragments of the present disclosure is 60 to 100%. In an embodiment, thewater solubility of pure silk fibroin-based protein fragments of thepresent disclosure is 70 to 100%. In an embodiment, the water solubilityof pure silk fibroin-based protein fragments of the present disclosureis 80 to 100%. In an embodiment, the water solubility is 90 to 100%. Inan embodiment, the silk fibroin-based fragments of the presentdisclosure are non-soluble in aqueous solutions.

In an embodiment, the solubility of pure silk fibroin-based proteinfragments of the present disclosure in organic solutions is 50 to 100%.In an embodiment, the solubility of pure silk fibroin-based proteinfragments of the present disclosure in organic solutions is 60 to 100%.In an embodiment, the solubility of pure silk fibroin-based proteinfragments of the present disclosure in organic solutions is 70 to 100%.In an embodiment, the solubility of pure silk fibroin-based proteinfragments of the present disclosure in organic solutions is 80 to 100%.In an embodiment, the solubility of pure silk fibroin-based proteinfragments of the present disclosure in organic solutions is 90 to 100%.In an embodiment, the silk fibroin-based fragments of the presentdisclosure are non-soluble in organic solutions.

In an embodiment, the percent water content in gels of the presentdisclosure is 20% to 99.9%. In an embodiment, the percent water contentin gels of the present disclosure is 20% to 25%. In an embodiment, thepercent water content in gels of the present disclosure is 25% to 30%.In an embodiment, the percent water content in gels of the presentdisclosure is 30% to 35%. In an embodiment, the percent water content ingels of the present disclosure is 35% to 40%. In an embodiment, thepercent water content in gels of the present disclosure is 40% to 45%.In an embodiment, the percent water content in gels of the presentdisclosure is 45% to 50%. in an embodiment, the percent water content ingels of the present disclosure is 50% to 55%. In an embodiment, thepercent water content in gels of the present disclosure is 55% to 60%.In an embodiment, the percent water content in gels of the presentdisclosure is 60% to 65%. In an embodiment, the percent water content ingels of the present disclosure is 65% to 70%. In an embodiment, thepercent water content in gels of the present disclosure is 70% to 75%.In an embodiment, the percent water content in gels of the presentdisclosure is 75% to 80%. In an embodiment, the percent water content ingels of the present disclosure is 80% to 85%. In an embodiment, thepercent water content in gels of the present disclosure is 85% to 90%.In an embodiment, the percent water content in gels of the presentdisclosure is 90% to 95%. In an embodiment, the percent water content ingels of the present disclosure is 95% to 99%.

In an embodiment, the percent water content in films of the presentdisclosure is 20%. In an embodiment, the percent water content in filmsof the present disclosure is less than 20%). In an embodiment, thepercent water content in films of the present disclosure is less than18%. In an embodiment, the percent water content in films of the presentdisclosure is less than 16%. In an embodiment, the percent water contentin films of the present disclosure is less than 14%. In an embodiment,the percent water content in films of the present disclosure is lessthan 12%. In an embodiment, the percent water content in films of thepresent disclosure is less than 10%. In an embodiment, the percent watercontent in films of the present disclosure is between about 2% and about20%.

In an embodiment, the percent water content in moisturizing compositionsof the present disclosure is about 70% (w/v). In an embodiment, thepercent water content in moisturizing compositions of the presentdisclosure is about 75% (w/v). In an embodiment, the percent watercontent in moisturizing compositions of the present disclosure is about80% (w/v). In an embodiment, the percent water content in moisturizingcompositions of the present disclosure is less than 99% (w/v). In anembodiment, the percent water content in moisturizing compositions ofthe present disclosure is less than 95% (w/v). In an embodiment, thepercent water content in moisturizing compositions of the presentdisclosure is less than 90% (w/v). In an embodiment, the percent watercontent in moisturizing compositions of the present disclosure is lessthan 85% (w/v). In an embodiment, the percent water content inmoisturizing compositions of the present disclosure is less than 80%(w/v). In an embodiment, the percent water content in moisturizingcompositions of the present disclosure is less than 78% (w/v). In anembodiment, the percent water content in moisturizing compositions ofthe present disclosure is less than 75% (w/v). In an embodiment, thepercent water content in moisturizing compositions of the presentdisclosure is less than 73% (w/v). In an embodiment, the percent watercontent in moisturizing compositions of the present disclosure is lessthan 70% (w/v). In an embodiment, the percent water content inmoisturizing compositions of the present disclosure is between about 70%(w/v) and about 99% (w/v). In an embodiment, the percent water contentin films of the present disclosure is between about 70% (w/v) and about90% (w/v). In an embodiment, the percent water content in moisturizingcompositions of the present disclosure is between about 70% (w/v) andabout 80% (w/v).

In an embodiment, the percent silk protein fragments content inmoisturizing compositions of the present disclosure is about 0.02%(w/v). In an embodiment, the percent silk protein fragments content inmoisturizing compositions of the present disclosure is about 0.04%(w/v). In an embodiment, the percent silk protein fragments content inmoisturizing compositions of the present disclosure is about 0.06%(w/v). In an embodiment, the percent silk protein fragments content inmoisturizing compositions of the present disclosure is about 0.08%(w/v). In an embodiment, the percent silk protein fragments content inmoisturizing compositions of the present disclosure is about 0.1% (w/v).In an embodiment, the percent silk protein fragments content inmoisturizing compositions of the present disclosure is about 0.12%(w/v). In an embodiment, the percent silk protein fragments content inmoisturizing compositions of the present disclosure is about 0.14%(w/v). In an embodiment, the percent silk protein fragments content inmoisturizing compositions of the present disclosure is about 0.16%(w/v). In an embodiment, the percent silk protein fragments content inmoisturizing compositions of the present disclosure is about 0.18%(w/v). In an embodiment, the percent silk protein fragments content inmoisturizing compositions of the present disclosure is about 0.2% (w/v).In an embodiment, the percent silk protein fragments content inmoisturizing compositions of the present disclosure is less than 6%(w/v). In an embodiment, the percent silk protein fragments content inmoisturizing compositions of the present disclosure is less than 2%(w/v). In an embodiment, the percent silk protein fragments content inmoisturizing compositions of the present disclosure is less than 1%(w/v). In an embodiment, the percent silk protein fragments content inmoisturizing compositions of the present disclosure is less than 0.5%(w/v). In an embodiment, the percent silk protein fragments content inmoisturizing compositions of the present disclosure is less than 0.2%(w/v). In an embodiment, the percent silk protein fragments content inmoisturizing compositions of the present disclosure is less than 0.18%(w/v). In an embodiment, the percent silk protein fragments content inmoisturizing compositions of the present disclosure is less than 0.14%(w/v). In an embodiment, the percent silk protein fragments content inmoisturizing compositions of the present disclosure is less than 0.1%(w/v). In an embodiment, the percent silk protein fragments content inmoisturizing compositions of the present disclosure is between about0.001% (w/v) and about 6% (w/v). In an embodiment, the percent silkprotein fragments content in films of the present disclosure is betweenabout 0.01% (w/v) and about 2% (w/v). In an embodiment, the percent silkprotein fragments content in moisturizing compositions of the presentdisclosure is between about 0.06% (w/v) and about 0.2% (w/v).

In an embodiment, a solution of the present disclosure is used to createan article with microneedles by standard methods known to one in the artfor controlled delivery of molecules or therapeutic agents to or throughthe skin.

A method for preparing an aqueous solution of pure silk fibroin-basedprotein fragments having an average weight average molecular weightranging from about 6 kDa to about 16 kDa includes the steps of:degumming a silk source by adding the silk source to a boiling (100° C.)aqueous solution of sodium carbonate for a treatment time of betweenabout 30 minutes to about 60 minutes; removing sericin from the solutionto produce a silk fibroin extract comprising non-detectable levels ofsericin; draining the solution from the silk fibroin extract; dissolvingthe silk fibroin extract in a solution of lithium bromide having astarting temperature upon placement of the silk fibroin extract in thelithium bromide solution that ranges from about 60° C. to about 140° C.;maintaining the solution of silk fibroin-lithium bromide in an ovenhaving a temperature of about 140° C. for a period of at least 1 hour;removing the lithium bromide from the silk fibroin extract; andproducing an aqueous solution of silk protein fragments, the aqueoussolution comprising: fragments having an average weight averagemolecular weight ranging from about 6 kDa to about 16 kDa, and whereinthe aqueous solution of pure silk fibroin-based protein fragmentscomprises a polydispersity of between about 1.5 and about 3.0. Themethod may further comprise drying the silk fibroin extract prior to thedissolving step. The aqueous solution of pure silk fibroin-based proteinfragments may comprise lithium bromide residuals of less than 300 ppm asmeasured using a high-performance liquid chromatography lithium bromideassay. The aqueous solution of pure silk fibroin-based protein fragmentsmay comprise sodium carbonate residuals of less than 100 ppm as measuredusing a high-performance liquid chromatography sodium carbonate assay.The method may further comprise adding a therapeutic agent to theaqueous solution of pure silk fibroin-based protein fragments. Themethod may further comprise adding a molecule selected from one of anantioxidant or an enzyme to the aqueous solution of pure silkfibroin-based protein fragments. The method may further comprise addinga vitamin to the aqueous solution of pure silk fibroin-based proteinfragments. The vitamin may be vitamin C or a derivative thereof. Theaqueous solution of pure silk fibroin-based protein fragments may belyophilized. The method may further comprise adding an alpha hydroxyacid to the aqueous solution of pure silk fibroin-based proteinfragments. The alpha hydroxy acid may be selected from the groupconsisting of glycolic acid, lactic acid, tartaric acid and citric acid.The method may further comprise adding hyaluronic acid or its salt format a concentration of about 0.5% to about 10.0% to the aqueous solutionof pure silk fibroin-based protein fragments. The method may furthercomprise adding at least one of zinc oxide or titanium dioxide. A filmmay be fabricated from the aqueous solution of pure silk fibroin-basedprotein fragments produced by this method. The film may comprise fromabout 1.0 wt. % to about 50.0 wt. % of vitamin C or a derivativethereof. The film may have a water content ranging from about 2.0 wt. %to about 20.0 wt. %. The film may comprise from about 30.0 wt. % toabout 99.5 wt. % of pure silk fibroin-based protein fragments. A gel maybe fabricated from the aqueous solution of pure silk fibroin-basedprotein fragments produced by this method. The gel may comprise fromabout 0.5 wt. % to about 20.0 wt. % of vitamin C or a derivativethereof. The gel may have a silk content of at least 2% and a vitamincontent of at least 20%.

A method for preparing an aqueous solution of pure silk fibroin-basedprotein fragments having an average weight average molecular weightranging from about 17 kDa to about 38 kDa includes the steps of: addinga silk source to a boiling (100° C.) aqueous solution of sodiumcarbonate for a treatment time of between about 30 minutes to about 60minutes so as to result in degumming; removing sericin from the solutionto produce a silk fibroin extract comprising non-detectable levels ofsericin; draining the solution from the silk fibroin extract; dissolvingthe silk fibroin extract in a solution of lithium bromide having astarting temperature upon placement of the silk fibroin extract in thelithium bromide solution that ranges from about 80° C. to about 140° C.;maintaining the solution of silk fibroin-lithium bromide in a dry ovenhaving a temperature in the range between about 60° C. to about 100° C.for a period of at least 1 hour; removing the lithium bromide from thesilk fibroin extract; and producing an aqueous solution of pure silkfibroin-based protein fragments, wherein the aqueous solution of puresilk fibroin-based protein fragments comprises lithium bromide residualsof between about 10 ppm and about 300 ppm, wherein the aqueous solutionof silk protein fragments comprises sodium carbonate residuals ofbetween about 10 ppm and about 100 ppm, wherein the aqueous solution ofpure silk fibroin-based protein fragments comprises fragments having anaverage weight average molecular weight ranging from about 17 kDa toabout 38 kDa, and wherein the aqueous solution of pure silkfibroin-based protein fragments comprises a polydispersity of betweenabout 1.5 and about 3.0. The method may further comprise drying the silkfibroin extract prior to the dissolving step. The aqueous solution ofpure silk fibroin-based protein fragments may comprise lithium bromideresiduals of less than 300 ppm as measured using a high-performanceliquid chromatography lithium bromide assay. The aqueous solution ofpure silk fibroin-based protein fragments may comprise sodium carbonateresiduals of less than 100 ppm as measured using a high-performanceliquid chromatography sodium carbonate assay. The method may furthercomprise adding a therapeutic agent to the aqueous solution of pure silkfibroin-based protein fragments. The method may further comprise addinga molecule selected from one of an antioxidant or an enzyme to theaqueous solution of pure silk fibroin-based protein fragments. Themethod may further comprise adding a vitamin to the aqueous solution ofpure silk fibroin-based protein fragments. The vitamin may be vitamin Cor a derivative thereof. The aqueous solution of pure silk fibroin-basedprotein fragments may be lyophilized. The method may further compriseadding an alpha hydroxy acid to the aqueous solution of pure silkfibroin-based protein fragments. The alpha hydroxy acid may be selectedfrom the group consisting of glycolic acid, lactic acid, tartaric acidand citric acid. The method may further comprise adding hyaluronic acidor its salt form at a concentration of about 0.5% to about 10.0% to theaqueous solution of pure silk fibroin-based protein fragments. Themethod may further comprise adding at least one of zinc oxide ortitanium dioxide. A film may be fabricated from the aqueous solution ofpure silk fibroin-based protein fragments produced by this method. Thefilm may comprise from about 1.0 wt. % to about 50.0 wt. % of vitamin Cor a derivative thereof. The film may have a water content ranging fromabout 2.0 wt. % to about 20.0 wt. %. The film may comprise from about30.0 wt. % to about 99.5 wt. % of pure silk fibroin-based proteinfragments. A gel may be fabricated from the aqueous solution of puresilk fibroin-based protein fragments produced by this method. The gelmay comprise from about 0.5 wt. % to about 20.0 wt. % of vitamin C or aderivative thereof. The gel may have a silk content of at least 2% and avitamin content of at least 20%.

According to aspects illustrated herein, there is disclosed a method forpreparing an aqueous solution of pure silk fibroin-based proteinfragments having an average weight average molecular weight ranging fromabout 39 kDa to about 80 kDa, the method including the steps of: addinga silk source to a boiling (100° C.) aqueous solution of sodiumcarbonate for a treatment time of about 30 minutes so as to result indegumming; removing sericin from the solution to produce a silk fibroinextract comprising non-detectable levels of sericin; draining thesolution from the silk fibroin extract; dissolving the silk fibroinextract in a solution of lithium bromide having a starting temperatureupon placement of the silk fibroin extract in the lithium bromidesolution that ranges from about 80° C. to about 140° C.; maintaining thesolution of silk fibroin-lithium bromide in a dry oven having atemperature in the range between about 60° C. to about 100° C. for aperiod of at least 1 hour; removing the lithium bromide from the silkfibroin extract; and producing an aqueous solution of pure silkfibroin-based protein fragments, wherein the aqueous solution of puresilk fibroin-based protein fragments comprises lithium bromide residualsof between about 10 ppm and about 300 ppm, sodium carbonate residuals ofbetween about 10 ppm and about 100 ppm, fragments having an averageweight average molecular weight ranging from about 40 kDa to about 65kDa, and wherein the aqueous solution of pure silk fibroin-based proteinfragments comprises a polydispersity of between about 1.5 and about 3.0.The method may further comprise drying the silk fibroin extract prior tothe dissolving step. The aqueous solution of pure silk fibroin-basedprotein fragments may comprise lithium bromide residuals of less than300 ppm as measured using a high-performance liquid chromatographylithium bromide assay. The aqueous solution of pure silk fibroin-basedprotein fragments may comprise sodium carbonate residuals of less than100 ppm as measured using a high-performance liquid chromatographysodium carbonate assay.

The method may further comprise adding a therapeutic agent to theaqueous solution of pure silk fibroin-based protein fragments. Themethod may further comprise adding a molecule selected from one of anantioxidant or an enzyme to the aqueous solution of pure silkfibroin-based protein fragments. The method may further comprise addinga vitamin to the aqueous solution of pure silk fibroin-based proteinfragments. The vitamin may be vitamin C or a derivative thereof. Theaqueous solution of pure silk fibroin-based protein fragments may belyophilized. The method may further comprise adding an alpha hydroxyacid to the aqueous solution of pure silk fibroin-based proteinfragments. The alpha hydroxy acid may be selected from the groupconsisting of glycolic acid, lactic acid, tartaric acid and citric acid.The method may further comprise adding hyaluronic acid or its salt format a concentration of about 0.5% to about 10.0% to the aqueous solutionof pure silk fibroin-based protein fragments. The method may furthercomprise adding at least one of zinc oxide or titanium dioxide. A filmmay be fabricated from the aqueous solution of pure silk fibroin-basedprotein fragments produced by this method. The film may comprise fromabout 1.0 wt. % to about 50.0 wt. % of vitamin C or a derivativethereof. The film may have a water content ranging from about 2.0 wt. %to about 20.0 wt. %. The film may comprise from about 30.0 wt. % toabout 99.5 wt. % of pure silk fibroin-based protein fragments. A gel maybe fabricated from the aqueous solution of pure silk fibroin-basedprotein fragments produced by this method. The gel may comprise fromabout 0.5 wt. % to about 20.0 wt, % of vitamin C or a derivativethereof. The gel may have a silk content of at least 2% and a vitamincontent of at least 20%.

In an embodiment, the compositions of the invention include one or moreemollients. Examples of emollients that may be included in thecompositions of the invention are as follows:

-   -   (1) hydrocarbon oils and waxes such as mineral oil, petrolatum,        paraffin, ozokerite, microcrystalline wax, polyethylene,        squalene, and perhydrosqualene;    -   (2) silicone oils, such as dimethyl polysiloxanes, methylphenyl        polysiloxanes, water-soluble and alcohol-soluble silicone glycol        copolymers;    -   (3) acetoglyceride esters, such as acetylated monoglycerides;    -   (4) ethoxylated glycerides, such as ethoxylated glyceryl        monostearate;    -   (5) alkyl esters of fatty acids having 10 to 20 carbon atoms        such as alkyl esters, which may include hexyl laurate, isohexyl        laurate, isohexyl palmitate, isopropyl palmitate, decyl oleate,        isodecyl oleate, hexadecyl stearate, decyl stearate, isopropyl        isostearate, diisopropyl adipate, diisohexyl adipate,        dihexyldecyl adipate, diisopropyl sebacate, lauryl lactate,        myristyl lactate, and cetyl lactate, including methyl,        isopropyl, and butyl esters of fatty acids;    -   (6) alkenyl esters of fatty acids having 10 to 20 carbon atoms        such as oleyl myristate, oleyl stearate, and oleyl oleate;    -   (7) fatty acids having 10 to 20 carbon atoms such as pelargonic,        lauric, myristic, palmitic, stearic, isostearic, hydroxystearic,        oleic, linoleic, ricinoleic, arachidic, behenic, and erucic        acids; (8) fatty alcohols having 10 to 20 carbon atoms such as        lauryl, myristyl, cetyl, hexadecyl, stearyl, isostearyl,        hydroxystearyl, oleyl, ricinoleyl, behenyl, erucyl alcohols, and        2-octyl dodecanol;    -   (9) fatty alcohols ethers including ethoxylated fatty alcohols        of 10 to 20 carbon atoms such as the lauryl, cetyl, stearyl,        isostearyl, oelyl, and cholesterol alcohols having attached        thereto from 1 to 50 ethylene oxide groups or 1 to 50 propylene        oxide groups;    -   (10) ether-esters such as fatty acid esters of ethoxylated fatty        alcohols;    -   (11) lanolin and its derivatives such as lanolin oil, lanolin        wax, lanolin alcohols, lanolin fatty acids, isopropyl lanolate,        ethoxylated lanolin, ethoxylated lanolin alcohols, ethoxylated        cholesterol, propoxylated lanolin alcohols, acetylated lanolin,        acetylated lanolin alcohols, lanolin alcohols linoleate, lanolin        alcohols ricinoleate, acetate of lanolin alcohols ricinoleate,        acetate of ethoxylated alcohols-esters, hydrogenolysis of        lanolin, ethoxylated hydrogenated lanolin, ethoxylated sorbitol        lanolin, and liquid and semisolid lanolin absorption bases;    -   (12) polyhydric alcohols and polyether derivatives such as        propylene glycol, dipropylene glycol, polypropylene glycols 2000        and 4000, polyoxyethylene polyoxyethylene glycols,        polyoxypropylene polyoxyethylene glycols, glycerol, sorbitol,        ethoxylated sorbitol, hydroxypropyl sorbitol, polyethylene        glycols 200-6000, methoxy polyethylene glycols 350, 550, 750,        2000 and 5000, poly[ethylene oxide]homopolymers        (100,000-5,000,000), polyalkylene glycols and derivatives,        hexylene glycol (2-methyl-2,4-pentanediol), 1,3-butylene glycol,        1,2,6-hexanetriol, ethohexadiol USP (2-ethyl-1,3-hexanediol),        C15-C18 vicinal glycol, and polyoxypropylene derivatives of        trimethylolpropane;    -   (13) polyhydric alcohol esters including ethylene glycol mono-        and di-fatty acid esters, diethylene glycol mono- and di-fatty        acid esters, polyethylene glycol (200-6000) mono- and di-fatty        acid esters, propylene glycol mono- and di-fatty acid esters,        polypropylene glycol 2000 monooleate, polypropylene glycol 2000        monostearate, ethoxylated propylene glycol monostearate,        glyceryl mono- and di-fatty acid esters, polyglycerol poly-fatty        acid esters, ethoxylated glyceryl monostearate, 1,3-butylene        glycol monostearate, 1,3-butylene glycol distearate,        polyoxyethylene polyol fatty acid ester, sorbitan fatty acid        esters, and polyoxyethylene sorbitan fatty acid esters;    -   (14) wax esters such as beeswax, spermaceti, myristyl myristate,        and stearyl stearate;    -   (15) beeswax derivatives, such as polyoxyethylene sorbitol        beeswax which are reaction products of beeswax with ethoxylated        sorbitol of varying ethylene oxide content, forming a mixture of        ether-esters;    -   (16) vegetable waxes including carnauba and candelilla waxes;    -   (17) natural or essential oils, including, vegetable oil, citrus        oil, plant oil, fish oil, non-citrus fruit oil, nut oils, oils        having flavors, perfume or scents; vegetable oils may include        canola oil, corn oil, neem oil, olive oil, cottonseed oil,        coconut oil, fractionated coconut oil, palm oil, nut oils,        safflower oil, sesame oil, soybean oil, and sunflower oil; nut        oils can be peanut oil, almond oil, cashew oil, hazelnut oil,        macadamia oil, pecan oil, pine nut oil, pistachio oil, and        walnut oil; citrus oils may include grapefruit seed oil, lemon        oil, orange oil, sweet orange oil, tangerine oil, lime oil,        mandarin oil, and the like; other natural or essential oils may        include fish oil such as omega 3 oil, flaxseed oil (linseed        oil), apricot oil, avocado oil, carrot oil, cocoa butter oil,        coconut oil, fractionated coconut oil, hemp oil, papaya seed        oil, rice bran oil, shea butter oil, tea tree seed oil, and        wheat germ oil; additional natural or essential oils may include        lavender oil, rosemary oil, tung oil, jojoba oil, poppy seed        oil, shea butter, castor oil, mango oil, rose hip oil, tall oil;        and natural or essential oils may include chamomile oil,        cinnamon oil, citronella oil, eucalyptus oil, fennel seed oil,        jasmine oil, juniper berry oil, raspberry seed oil, lavender        oil, primrose oil, lemon grass oil, nutmeg oil, patchouli oil,        peppermint oil, pine oil, rose oil, rose hip oil, rosemary oil,        eucalyptus oil, tea tree oil, rosewood oil, sandalwood oil,        sassafras oil, spearmint oil, and wintergreen oil;    -   (18) phospholipids, such as lecithin and derivatives;    -   (19) sterols such as cholesterol and cholesterol fatty acid        esters; and    -   (20) amides such as fatty acid amides, ethoxylated fatty acid        amides, and solid fatty acid alkanolamides. Examples of        emollients that may be included in the compositions of the        invention may include one or more of ricinus communis (castor)        seed oil, lanolin, aloe barbadensis leaf extract, therbroma        cacao (cocoa) seed butter, petrolatum, euphorbia cerifera        (candelilla) wax, honey, gerniol, menthol, camphor, cetyl        esters, mineral oil, salicylic acid, lavandula angustifolia        (lavender) flower extract, phenol, olea europaea (olive) oil,        camellia sinensis (green tea) seed oil, prunus armeniacea (acai)        fruit oil, persea gratissima (avocado) oil, vegetable oil,        palmitoyl isoleucine, sambucus nigra (elderberry) fruit extract,        phoenix dactylifera (date) seed extract, avandula stoechas        (spanish lavender) exract, spiraea ulmaria (meadowsweet) leave        extract, chamomilla recutita (chamomile) leaf extract, and        symphytum officinale (comfrey) leaf extract.

In some embodiments, the compositions of the invention may include oneor more emollients that may be in an amount of about 50 wt. %, about 45wt. %, about 40 wt. %, about 35 wt. %, about 30 wt. %, about 25 wt. %,about 20 wt. %, about 19.75 wt. %, about 19.50 wt. %, about 19.25 wt. %,about 19 wt. %, about 18.75 wt. %, about 18.50 wt. %, about 18.25 wt. %,about 18 wt. %, about 17.75 wt. %, about 17.50 wt. %, about 17.25 wt. %,about 17 wt. %, about 16.75 wt. %, about 16.50 wt. %, about 16.25 wt. %about 16 wt. %, about 15.75 wt. %, about 15.50 wt. %, about 15.25 wt. %,about 15 wt. %, about 14.75 wt. %, about 14.50 wt. %, about 14.25 wt. %,about 14 wt. %, about 13.75 wt. %, about 13.50 wt. %, about 13.25 wt. %,about 13 wt. %, about 12.75 wt. %, about 12.50 wt. %, about 12.25 wt. %,about 12 wt. %, about 11.75 wt. %, about 11.50 wt. %, about 11.25 wt. %,about 11 wt. %, about 10.75 wt. %, about 10.50 wt. %, about 10.25 wt. %,about 10 wt. %, about 9.75 wt. %, about 9.50 wt. %, about 9.25 wt. %,about 9 wt. %, about 8.75 wt. %, about 8.50 wt. %, about 8.25 wt. %,about 8 wt. %, about 7.75 wt. %, about 7.50 wt. %, about 7.25 wt. %,about 7 wt. %, about 6.75 wt. %, about 6.50 wt. %, about 6.25 wt. %,about 6 wt. %, about 5.75 wt. %, about 5.50 wt. %, about 5.25 wt. %,about 5 wt. %, about 4.75 wt. %, about 4.50 wt. %, about 4.25 wt. %,about 4 wt. %, about 3.75 wt. %, about 3.50 wt. %, about 3.25 wt. %,about 3 wt. %, about 2.75 wt. %, about 2.50 wt. %, about 2.25 wt. %,about 2 wt. %, about 1.75 wt. %, about 1.50 wt. %, about 1.25 wt. %,about 1 wt. %, about 0.5 wt. %, about 0.4 wt. %, about 0.3 wt. %, about0.2 wt. %, about 0.1 wt. %, about 0.09 wt. %, about 0.08 wt. %, about0.07 wt. %, about 0.06 wt. %, about 0.05 wt. %, about 0.04 wt. %, about0.03 wt. %, about 0.02 wt. %, about 0.01 wt. %, about 0.009 wt. %, about0.008 wt. %, about 0.007 wt. %, about 0.006 wt. %, about 0.005 wt. %,about 0.004 wt. %, about 0.003 wt. %, about 0.002 wt. %, or about 0.001wt. %.

In some embodiments, the compositions of the invention may include oneor more emollients that may be in an amount of between about 1 wt. % toabout 50 wt. %, between about 2 wt. % to about 40 wt. %, between about 3wt. % to about 30 wt. %, between about 4 wt. % to about 20 wt. %,between about 5 wt. % to about 15 wt. %, between about 6 wt. % to about10 wt. %, between about 7 wt. % to about 9 wt. %, between about 10 wt. %to about 50 wt. %, between about 15 wt. % to about 45 wt. %, betweenabout 20 wt. % to about 40 wt. %, between about 25 wt. % to about 35 wt.%, or between about 25 wt. % to about 30 wt. %.

In some embodiments, the compositions of the invention may include oneor more emollients that may be in an amount of between about 0.001 wt. %to about 5 wt. %, between about 5 wt. % to about 10 wt. %, between about10 wt. % to about 15 wt. %, between about 15 wt. % to about 20 wt. %,between about 20 wt. % to about 25 wt. %, between about 25 wt. % toabout 30 wt. %, between about 30 wt. % to about 35 wt. %, between about35 wt. % to about 40 wt. %, between about 40 wt. % to about 45 wt. %, orbetween about 45 wt. % to about 50 wt. %.

In some embodiments, the compositions of the invention may include oneor more emollients that may be in an amount of between about 0.001 wt. %to about 1 wt. %, between about 1 wt. % to about 2 wt. %, between about2 wt. % to about 3 wt. %, between about 3 wt. % to about 4 wt. %,between about 4 wt. % to about 5 wt. %, between about 5 wt. % to about 6wt. %, between about 6 wt. % to about 7 wt. %, between about 7 wt. % toabout 8 wt. %, between about 8 wt. % to about 9 wt. %, between about 9wt. % to about 10 wt. %, between about 10 wt. % to about 11 wt. %,between about 11 wt. % to about 12 wt. %, between about 12 wt. % toabout 13 wt. %, between about 13 wt. % to about 14 wt. %, between about14 wt. % to about 15 wt. %, between about 15 wt. % to about 16 wt. %,between about 16 wt. % to about 17 wt. %, between about 17 wt. % toabout 18 wt. %, between about 18 wt. % to about 19 wt. %, between about19 wt. % to about 20 wt. %, between about 20 wt. % to about 21 wt. %,between about 21 wt. % to about 22 wt. %, between about 22 wt. % toabout 23 wt. %, between about 23 wt. % to about 24 wt. %, between about24 wt. % to about 25 wt. %, between about 25 wt. % to about 26 wt. %,between about 26 wt. % to about 27 wt. %, between about 27 wt. % toabout 28 wt. %, between about 28 wt. % to about 29 wt. %, between about29 wt. % to about 30 wt. %, between about 30 wt. % to about 31 wt. %,between about 31 wt. % to about 32 wt. %, between about 32 wt. % toabout 33 wt. %, between about 33 wt. % to about 34 wt. %, between about34 wt. % to about 35 wt. %, between about 35 wt. % to about 36 wt. %,between about 36 wt. % to about 37 wt. %, between about 37 wt. % toabout 38 wt. %, between about 38 wt. % to about 39 wt. %, between about39 wt. % to about 40 wt. %, between about 40 wt. % to about 41 wt. %,between about 41 wt. % to about 42 wt. %, between about 42 wt. % toabout 43 wt. %, between about 43 wt. % to about 44 wt. %, between about44 wt. % to about 45 wt. %, between about 45 wt. % to about 46 wt. %,between about 46 wt. % to about 47 wt. %, between about 47 wt. % toabout 48 wt. %, between about 48 wt. % to about 49 wt. %, or betweenabout 49 wt. % to about 50 wt. %.

In some embodiments, the compositions of the invention may include oneor more emollients that may be in an amount of about 50 wt. %, 45 wt. %,40 wt. %, 35 wt. %, 30 wt. %, 25 wt. %, 20 wt. %, 19.75 wt. %, 19.50 wt.%, 19.25 wt. %, 19 wt. %, 18.75 wt. %, 18.50 wt. %, 18.25 wt. %, 18 wt.%, 17.75 wt. %, 17.50 wt. %, 17.25 wt. %, 17 wt. %, 16.75 wt. %, 16.50wt. %, 16.25 wt. % 16 wt. %, 15.75 wt. %, 15.50 wt. %, 15.25 wt. %, 15wt. %, 14.75 wt. %, 14.50 wt. %, 14.25 wt. %, 14 wt. %, 13.75 wt. %,13.50 wt. %, 13.25 wt. %, 13 wt. %, 12.75 wt. %, 12.50 wt. %, 12.25 wt.%, 12 wt. %, 11.75 wt. %, 11.50 wt. %, 11.25 wt. %, 11 wt. %, 10.75 wt.%, 10.50 wt. %, 10.25 wt. %, 10 wt. %, 9.75 wt. %, 9.50 wt. %, 9.25 wt.%, 9 wt. %, 8.75 wt. %, 8.50 wt. %, 8.25 wt. %, 8 wt. %, 7.75 wt. %,7.50 wt. %, 7.25 wt. %, 7 wt. %, 6.75 wt. %, 6.50 wt. %, 6.25 wt. %, 6wt. %, 5.75 wt. %, 5.50 wt. %, 5.25 wt. %, 5 wt. %, 4.75 wt. %, 4.50 wt.%, 4.25 wt. %, 4 wt. %, 3.75 wt. %, 3.50 wt. %, 3.25 wt. %, 3 wt. %,2.75 wt. %, 2.50 wt. %, 2.25 wt. %, 2 wt. %, 1.75 wt. %, 1.50 wt. %,1.25 wt. %, 1 wt. %, 0.5 wt. %, 0.4 wt. %, 0.3 wt. %, 0.2 wt. %, 0.1 wt.%, 0.09 wt. %, 0.08 wt. %, 0.07 wt. %, 0.06 wt. %, 0.05 wt. %, 0.04 wt.%, 0.03 wt. %, 0.02 wt. %, 0.01 wt. %, 0.009 wt. %, 0.008 wt. %, 0.007wt. %, 0.006 wt. %, 0.005 wt. %, 0.004 wt. %, 0.003 wt. %, 0.002 wt. %,or 0.001 wt. %.

In some embodiments, the compositions of the invention may include oneor more emollients that may be in an amount of about between 1 wt. % to50 wt. %, between 2 wt. % to 40 wt. %, between 3 wt. % to 30 wt. %,between 4 wt. % to 20 wt. %, between 5 wt. % to 15 wt. %, between 6 wt.% to 10 wt. %, between 7 wt. % to 9 wt. %, between 10 wt. % to 50 wt. %,between 15 wt. % to 45 wt. %, between 20 wt. % to 40 wt. %, between 25wt. % to 35 wt. %, or between 30 wt. % to 35 wt. %.

In some embodiments, the compositions of the invention may include oneor more emollients that may be in an amount of about between 0.001 wt. %to 5 wt. %, between 5 wt. % to 10 wt. %, between 10 wt. % to 15 wt. %,between 15 wt. % to 20 wt. %, between 20 wt. % to 25 wt. %, between 25wt. % to 30 wt. %, between 30 wt. % to 35 wt. %, between 35 wt. % to 40wt. %, between 40 wt. % to 45 wt. %, or between 45 wt. % to 50 wt. %.

In some embodiments, the compositions of the invention may include oneor more emollients that may be in an amount of about between 0.001 wt. %to 1 wt. %, between 1 wt. % to 2 wt. %, between 2 wt. % to 3 wt. %,between 3 wt. % to 4 wt. %, between 4 wt. % to 5 wt. %, between 5 wt. %to 6 wt. %, between 6 wt. % to 7 wt. %, between 7 wt. % to 8 wt. %,between 8 wt. % to 9 wt. %, between 9 wt. % to 10 wt. %, between 10 wt.% to 11 wt. %, between 11 wt. % to 12 wt. %, between 12 wt. % to 13 wt.%, between 13 wt. % to 14 wt. %, between 14 wt. % to 15 wt. %, between15 wt. % to 16 wt. %, between 16 wt. % to 17 wt. %, between 17 wt. % to18 wt. %, between 18 wt. % to 19 wt. %, between 19 wt. % to 20 wt. %,between 20 wt. % to 21 wt. %, between 21 wt. % to 22 wt. %, between 22wt. % to 23 wt. %, between 23 wt. % to 24 wt. %, between 24 wt. % to 25wt. %, between 25 wt. % to 26 wt. %, between 26 wt. % to 27 wt. %,between 27 wt. % to 28 wt. %, between 28 wt. % to 29 wt. %, between 29wt. % to 30 wt. %, between 30 wt. % to 31 wt. %, between 31 wt. % to 32wt. %, between 32 wt. % to 33 wt. %, between 33 wt. % to 34 wt. %,between 34 wt. % to 35 wt. %, between 35 wt. % to 36 wt. %, between 36wt. % to 37 wt. %, between 37 wt. % to 38 wt. %, between 38 wt. % to 39wt. %, between 39 wt. % to 40 wt. %, between 40 wt. % to 41 wt. %,between 41 wt. % to 42 wt. %, between 42 wt. % to 43 wt. %, between 43wt. % to 44 wt. %, between 44 wt. % to 45 wt. %, between 45 wt. % to 46wt. %, between 46 wt. % to 47 wt. %, between 47 wt. % to 48 wt. %,between 48 wt. % to 49 wt. %, or between 49 wt. % to 50 wt. %.

In some embodiments, the compositions of the invention may include oneor more emollients that may be in an amount of about less than 50 wt. %,less than 40 wt. %, less than 30 wt. %, less than 20 wt. %, less than19.75 wt. %, less than 19.50 wt. %, less than 19.25 wt. %, less than 19wt. %, less than 18.75 wt. %, less than 18.50 wt. %, less than 18.25 wt.%, less than 18 wt. %, less than 17.75 wt. %, less than 17.50 wt. %,less than 17.25 wt. %, less than 17 wt. %, less than 16.75 wt. %, lessthan 16.50 wt. %, less than 16.25 wt. % less than 16 wt. %, less than15.75 wt. %, less than 15.50 wt. %, less than 15.25 wt. %, less than 15wt. %, less than 14.75 wt. %, less than 14.50 wt. %, less than 14.25 wt.%, less than 14 wt. %, less than 13.75 wt. %, less than 13.50 wt. %,less than 13.25 wt. %, less than 13 wt. %, less than 12.75 wt. %, lessthan 12.50 wt. %, less than 12.25 wt. %, less than 12 wt. %, less than11.75 wt. %, less than 11.50 wt. %, less than 11.25 wt. %, less than 11wt. %, less than 10.75 wt. %, less than 10.50 wt. %, less than 10.25 wt.%, less than 10 wt. %, less than 9.75 wt. %, less than 9.50 wt. %, lessthan 9.25 wt. %, less than 9 wt. %, less than 8.75 wt. %, less than 8.50wt. %, less than 8.25 wt. %, less than 8 wt. %, less than 7.75 wt. %,less than 7.50 wt. %, less than 7.25 wt. %, less than 7 wt. %, less than6.75 wt. %, less than 6.50 wt. %, less than 6.25 wt. %, less than 6 wt.%, less than 5.75 wt. %, less than 5.50 wt. %, less than 5.25 wt. %,less than 5 wt. %, less than 4.75 wt. %, less than 4.50 wt. %, less than4.25 wt. %, less than 4 wt. %, less than 3.75 wt. %, less than 3.50 wt.%, less than 3.25 wt. %, less than 3 wt. %, less than 2.75 wt. %, lessthan 2.50 wt. %, less than 2.25 wt. %, less than 2 wt. %, less than 1.75wt. %, less than 1.50 wt. %, less than 1.25 wt. %, less than 1 wt. %,less than 0.5 wt. %, less than 0.4 wt. %, less than 0.3 wt. %, less than0.2 wt. %, less than 0.1 wt. %, less than 0.09 wt. %, less than 0.08 wt.%, less than 0.07 wt. %, less than 0.06 wt. %, less than 0.05 wt. %,less than 0.04 wt. %, less than 0.03 wt. %, less than 0.02 wt. %, lessthan 0.01 wt. %, less than 0.009 wt. %, less than 0.008 wt. %, less than0.007 wt. %, less than 0.006 wt. %, less than 0.005 wt. %, less than0.004 wt. %, less than 0.003 wt. %, less than 0.002 wt. %, or less than0.001 wt. %.

In some embodiments, the compositions of the invention may include oneor more emollients that may be in an amount of about greater than 45 wt.%, greater than 40 wt. %, greater than 30 wt. %, greater than 20 wt. %,greater than 19.75 wt. %, greater than 19.50 wt. %, greater than 19.25wt. %, greater than 19 wt. %, greater than 18.75 wt. %, greater than18.50 wt. %, greater than 18.25 wt. %, greater than 18 wt. %, greaterthan 17.75 wt. %, greater than 17.50 wt. %, greater than 17.25 wt. %,greater than 17 wt. %, greater than 16.75 wt. %, greater than 16.50 wt.%, greater than 16.25 wt. % greater than 16 wt. %, greater than 15.75wt. %, greater than 15.50 wt. %, greater than 15.25 wt. %, greater than15 wt. %, greater than 14.75 wt. %, greater than 14.50 wt. %, greaterthan 14.25 wt. %, greater than 14 wt. %, greater than 13.75 wt. %,greater than 13.50 wt. %, greater than 13.25 wt. %, greater than 13 wt.%, greater than 12.75 wt. %, greater than 12.50 wt. %, greater than12.25 wt. %, greater than 12 wt. %, greater than 11.75 wt. %, greaterthan 11.50 wt. %, greater than 11.25 wt. %, greater than 11 wt. %,greater than 10.75 wt. %, greater than 10.50 wt. %, greater than 10.25wt. %, greater than 10 wt. %, greater than 9.75 wt. %, greater than 9.50wt. %, greater than 9.25 wt. %, greater than 9 wt. %, greater than 8.75wt. %, greater than 8.50 wt. %, greater than 8.25 wt. %, greater than 8wt. %, greater than 7.75 wt. %, greater than 7.50 wt. %, greater than7.25 wt. %, greater than 7 wt. %, greater than 6.75 wt. %, greater than6.50 wt. %, greater than 6.25 wt. %, greater than 6 wt. %, greater than5.75 wt. %, greater than 5.50 wt. %, greater than 5.25 wt. %, greaterthan 5 wt. %, greater than 4.75 wt. %, greater than 4.50 wt. %, greaterthan 4.25 wt. %, greater than 4 wt. %, greater than 3.75 wt. %, greaterthan 3.50 wt. %, greater than 3.25 wt. %, greater than 3 wt. %, greaterthan 2.75 wt. %, greater than 2.50 wt. %, greater than 2.25 wt. %,greater than 2 wt. %, greater than 1.75 wt. %, greater than 1.50 wt. %,greater than 1.25 wt. %, greater than 1 wt. %, greater than 0.5 wt. %,greater than 0.4 wt. %, greater than 0.3 wt. %, greater than 0.2 wt. %,greater than 0.1 wt. %, greater than 0.09 wt. %, greater than 0.08 wt.%, greater than 0.07 wt. %, greater than 0.06 wt. %, greater than 0.05wt. %, greater than 0.04 wt. %, greater than 0.03 wt. %, greater than0.02 wt. %, greater than 0.01 wt. %, greater than 0.009 wt. %, greaterthan 0.008 wt. %, greater than 0.007 wt. %, greater than 0.006 wt. %,greater than 0.005 wt. %, greater than 0.004 wt. %, greater than 0.003wt. %, greater than 0.002 wt. %, or greater than 0.001 wt. %.

In some embodiments, the compositions of the invention may include oneor more preservatives. For example, the preservatives used in theinvention may include Dermofeel PA-3 (water, ethanol, sodium phytate),sodium phytate, glyceryl caprylate, or caprylic/capric triglycerides.

In some embodiments, the compositions of the invention may include ascent. For example, the scent may be provided by one or more of theemollients or a synthetic scent or flavoring agent, including, withoutlimitation, mint (e.g., peppermint essential oil and/or spearmintessential oil), orange (e.g., sweet orange essential oil and/or orangeoil), or unscented (e.g., rosehip oil).

Moisturizer Compositions and Methods

In an embodiment, the percent hyaluronic acid content in moisturizingcompositions of the present disclosure is about 0.1% (w/v). In anembodiment, the percent hyaluronic acid content in moisturizingcompositions of the present disclosure is about 1% (w/v). In anembodiment, the percent hyaluronic acid content in moisturizingcompositions of the present disclosure is about 1.3% (w/v). In anembodiment, the percent hyaluronic acid content in moisturizingcompositions of the present disclosure is about 1.5% (w/v). In anembodiment, the percent hyaluronic acid content in moisturizingcompositions of the present disclosure is about 1.8% (w/v). In anembodiment, the percent hyaluronic acid content in moisturizingcompositions of the present disclosure is about 2% (w/v). In anembodiment, the percent hyaluronic acid content in moisturizingcompositions of the present disclosure is about 3% (w/v). In anembodiment, the percent hyaluronic acid content in moisturizingcompositions of the present disclosure is about 4% (w/v). In anembodiment, the percent hyaluronic acid content in moisturizingcompositions of the present disclosure is about 5% (w/v). In anembodiment, the percent hyaluronic acid content in moisturizingcompositions of the present disclosure is less than 5% (w/v). In anembodiment, the percent hyaluronic acid content in moisturizingcompositions of the present disclosure is less than 4% (w/v). In anembodiment, the percent hyaluronic acid content in moisturizingcompositions of the present disclosure is less than 3% (w/v). In anembodiment, the percent hyaluronic acid content in moisturizingcompositions of the present disclosure is less than 2% (w/v). In anembodiment, the percent hyaluronic acid content in moisturizingcompositions of the present disclosure is less than 1.5% (w/v). In anembodiment, the percent hyaluronic acid content in moisturizingcompositions of the present disclosure is less than 1% (w/v). In anembodiment, the percent hyaluronic acid content in moisturizingcompositions of the present disclosure is less than 0.5% (w/v). In anembodiment, the percent hyaluronic acid content in moisturizingcompositions of the present disclosure is less than 0.1% (w/v). In anembodiment, the percent hyaluronic acid content in moisturizingcompositions of the present disclosure is between about 0.1% (w/v) andabout 5% (w/v). In an embodiment, the percent hyaluronic acid content infilms of the present disclosure is between about 0.5% (w/v) and about 3%(w/v). In an embodiment, the percent hyaluronic acid content inmoisturizing compositions of the present disclosure is between about 1%(w/v) and about 2% (w/v). Alternatively, in some embodiments, thecompositions of the invention may exclude hyaluronic acid.

In some embodiments, a moisturizing composition of the presentcomposition comprises an oil or butter, for example, jojoba oil, rosehipoil, coconut oil, lemongrass oil, shea butter, glycerin, or acombination of two or more thereof. In an embodiment, the percentcontent of each oil or butter, (e.g., jojoba oil, rosehip oil, coconutoil, lemongrass oil, shea butter, or glycerin) in moisturizingcompositions of the present disclosure is about 1% (v/v). In anembodiment, the percent content of each oil or butter, (e.g., jojobaoil, rosehip oil, coconut oil, lemongrass oil, shea butter, or glycerin)in moisturizing compositions of the present disclosure is about 5%(v/v). In an embodiment, the percent content of each oil or butter,(e.g., jojoba oil, rosehip oil, coconut oil, lemongrass oil, sheabutter, or glycerin) in moisturizing compositions of the presentdisclosure is about 10% (v/v). In an embodiment, the percent content ofeach oil or butter, (e.g., jojoba oil, rosehip oil, coconut oil,lemongrass oil, shea butter, or glycerin) in moisturizing compositionsof the present disclosure is about 15% (v/v). In an embodiment, thepercent content of each oil or butter, (e.g., jojoba oil, rosehip oil,coconut oil, lemongrass oil, shea butter, or glycerin) in moisturizingcompositions of the present disclosure is about 20% (v/v). In anembodiment, the percent content of each oil or butter, (e.g., jojobaoil, rosehip oil, coconut oil, lemongrass oil, shea butter, or glycerin)in moisturizing compositions of the present disclosure is about 25%(v/v). In an embodiment, the percent content of each oil or butter,(e.g., jojoba oil, rosehip oil, coconut oil, lemongrass oil, sheabutter, or glycerin) in moisturizing compositions of the presentdisclosure is less than 25% (v/v). In an embodiment, the percent contentof each oil or butter, (e.g., jojoba oil, rosehip oil, coconut oil,lemongrass oil, shea butter, or glycerin) in moisturizing compositionsof the present disclosure is less than 20% (v/v). In an embodiment, thepercent content of each oil or butter, (e.g., jojoba oil, rosehip oil,coconut oil, lemongrass oil, shea butter, or glycerin) in moisturizingcompositions of the present disclosure is less than 15% (v/v). In anembodiment, the percent content of each oil or butter, (e.g., jojobaoil, rosehip oil, coconut oil, lemongrass oil, shea butter, or glycerin)in moisturizing compositions of the present disclosure is less than 10%(v/v). In an embodiment, the percent content of each oil or butter,(e.g., jojoba oil, rosehip oil, coconut oil, lemongrass oil, sheabutter, or glycerin) in moisturizing compositions of the presentdisclosure is less than 5% (v/v). In an embodiment, the percent contentof each oil or butter, (e.g., jojoba oil, rosehip oil, coconut oil,lemongrass oil, shea butter, or glycerin) in moisturizing compositionsof the present disclosure is less than 1% (v/v). In an embodiment, thepercent content of each oil or butter, (e.g., jojoba oil, rosehip oil,coconut oil, lemongrass oil, shea butter, or glycerin) in moisturizingcompositions of the present disclosure is between 0% (v/v) and 25%(v/v). In an embodiment, the percent content of each oil or butter,(e.g., jojoba oil, rosehip oil, coconut oil, lemongrass oil, sheabutter, or glycerin) in moisturizing compositions of the presentdisclosure is between 0.1% (v/v) and 25% (v/v). In an embodiment, thepercent content of each oil or butter, (e.g., jojoba oil, rosehip oil,coconut oil, lemongrass oil, shea butter, or glycerin) in moisturizingcompositions of the present disclosure is between 1% (v/v) and 20%(v/v). In an embodiment, the percent content of each oil or butter,(e.g., jojoba oil, rosehip oil, coconut oil, lemongrass oil, sheabutter, or glycerin) in moisturizing compositions of the presentdisclosure is between 5% (v/v) and 15% (v/v).

In an embodiment, the percent jojoba oil content in moisturizingcompositions of the present disclosure is about 1% (v/v). In anembodiment, the percent jojoba oil content in moisturizing compositionsof the present disclosure is about 5% (v/v). In an embodiment, thepercent jojoba oil content in moisturizing compositions of the presentdisclosure is about 10% (v/v). In an embodiment, the percent jojoba oilcontent in moisturizing compositions of the present disclosure is about15% (v/v). In an embodiment, the percent jojoba oil content inmoisturizing compositions of the present disclosure is about 20% (v/v).In an embodiment, the percent jojoba oil content in moisturizingcompositions of the present disclosure is about 25% (v/v). In anembodiment, the percent jojoba oil content in moisturizing compositionsof the present disclosure is less than 25% (v/v). In an embodiment, thepercent jojoba oil content in moisturizing compositions of the presentdisclosure is less than 20% (v/v). In an embodiment, the percent jojobaoil content in moisturizing compositions of the present disclosure isless than 15% (v/v). In an embodiment, the percent jojoba oil content inmoisturizing compositions of the present disclosure is less than 10%(v/v). In an embodiment, the percent jojoba oil content in moisturizingcompositions of the present disclosure is less than 5% (v/v). In anembodiment, the percent jojoba oil content in moisturizing compositionsof the present disclosure is less than 1% (v/v). In an embodiment, thepercent jojoba oil content in moisturizing compositions of the presentdisclosure is between 0% (v/v) and 25% (v/v). In an embodiment, thepercent jojoba oil content in moisturizing compositions of the presentdisclosure is between 0.1% (v/v) and 25% (v/v). In an embodiment, thepercent jojoba oil content in moisturizing compositions of the presentdisclosure is between 1% (v/v) and 20% (v/v). In an embodiment, thepercent jojoba oil content in moisturizing compositions of the presentdisclosure is between 5% (v/v) and 15% (v/v).

In an embodiment, the percent rosehip oil content in moisturizingcompositions of the present disclosure is about 1% (v/v). In anembodiment, the percent rosehip oil content in moisturizing compositionsof the present disclosure is about 5% (v/v). In an embodiment, thepercent rosehip oil content in moisturizing compositions of the presentdisclosure is about 10% (v/v). In an embodiment, the percent rosehip oilcontent in moisturizing compositions of the present disclosure is about15% (v/v). In an embodiment, the percent rosehip oil content inmoisturizing compositions of the present disclosure is about 20% (v/v).In an embodiment, the percent rosehip oil content in moisturizingcompositions of the present disclosure is about 25% (v/v). In anembodiment, the percent rosehip oil content in moisturizing compositionsof the present disclosure is less than 25% (v/v). In an embodiment, thepercent rosehip oil content in moisturizing compositions of the presentdisclosure is less than 20% (v/v). In an embodiment, the percent rosehipoil content in moisturizing compositions of the present disclosure isless than 15% (v/v). In an embodiment, the percent rosehip oil contentin moisturizing compositions of the present disclosure is less than 10%(v/v). In an embodiment, the percent rosehip oil content in moisturizingcompositions of the present disclosure is less than 5% (v/v). In anembodiment, the percent rosehip oil content in moisturizing compositionsof the present disclosure is less than 1% (v/v). In an embodiment, thepercent rosehip oil content in moisturizing compositions of the presentdisclosure is between 0% (v/v) and 25% (v/v). In an embodiment, thepercent rosehip oil content in moisturizing compositions of the presentdisclosure is between 0.1% (v/v) and 25% (v/v). In an embodiment, thepercent rosehip oil content in moisturizing compositions of the presentdisclosure is between 1% (v/v) and 20% (v/v). In an embodiment, thepercent rosehip oil content in moisturizing compositions of the presentdisclosure is between 5% (v/v) and 15% (v/v).

In an embodiment, the percent coconut oil content in moisturizingcompositions of the present disclosure is about 1% (v/v). In anembodiment, the percent coconut oil content in moisturizing compositionsof the present disclosure is about 5% (v/v). In an embodiment, thepercent coconut oil content in moisturizing compositions of the presentdisclosure is about 10% (v/v). In an embodiment, the percent coconut oilcontent in moisturizing compositions of the present disclosure is about15% (v/v). In an embodiment, the percent coconut oil content inmoisturizing compositions of the present disclosure is about 20% (v/v).In an embodiment, the percent coconut oil content in moisturizingcompositions of the present disclosure is about 25% (v/v). In anembodiment, the percent coconut oil content in moisturizing compositionsof the present disclosure is less than 25% (v/v). In an embodiment, thepercent coconut oil content in moisturizing compositions of the presentdisclosure is less than 20% (v/v). In an embodiment, the percent coconutoil content in moisturizing compositions of the present disclosure isless than 15% (v/v). In an embodiment, the percent coconut oil contentin moisturizing compositions of the present disclosure is less than 10%(v/v). In an embodiment, the percent coconut oil content in moisturizingcompositions of the present disclosure is less than 5% (v/v). In anembodiment, the percent coconut oil content in moisturizing compositionsof the present disclosure is less than 1% (v/v). In an embodiment, thepercent coconut oil content in moisturizing compositions of the presentdisclosure is between 0% (v/v) and 25% (v/v). In an embodiment, thepercent coconut oil content in moisturizing compositions of the presentdisclosure is between 0.1% (v/v) and 25% (v/v). In an embodiment, thepercent coconut oil content in moisturizing compositions of the presentdisclosure is between 1% (v/v) and 20% (v/v). In an embodiment, thepercent coconut oil content in moisturizing compositions of the presentdisclosure is between 5% (v/v) and 15% (v/v).

In an embodiment, the percent lemongrass oil content in moisturizingcompositions of the present disclosure is about 1% (v/v). In anembodiment, the percent lemongrass oil content in moisturizingcompositions of the present disclosure is about 5% (v/v). In anembodiment, the percent lemongrass oil content in moisturizingcompositions of the present disclosure is about 10% (v/v). In anembodiment, the percent lemongrass oil content in moisturizingcompositions of the present disclosure is about 15% (v/v). In anembodiment, the percent lemongrass oil content in moisturizingcompositions of the present disclosure is about 20% (v/v). In anembodiment, the percent lemongrass oil content in moisturizingcompositions of the present disclosure is about 25% (v/v). In anembodiment, the percent lemongrass oil content in moisturizingcompositions of the present disclosure is less than 25% (v/v). In anembodiment, the percent lemongrass oil content in moisturizingcompositions of the present disclosure is less than 20% (v/v). In anembodiment, the percent lemongrass oil content in moisturizingcompositions of the present disclosure is less than 15% (v/v). In anembodiment, the percent lemongrass oil content in moisturizingcompositions of the present disclosure is less than 10% (v/v). In anembodiment, the percent lemongrass oil content in moisturizingcompositions of the present disclosure is less than 5% (v/v). In anembodiment, the percent lemongrass oil content in moisturizingcompositions of the present disclosure is less than 1% (v/v). In anembodiment, the percent lemongrass oil content in moisturizingcompositions of the present disclosure is between 0% (v/v) and 25%(v/v). In an embodiment, the percent lemongrass oil content inmoisturizing compositions of the present disclosure is between 0.1%(v/v) and 25% (v/v). In an embodiment, the percent lemongrass oilcontent in moisturizing compositions of the present disclosure isbetween 1% (v/v) and 20% (v/v). In an embodiment, the percent lemongrassoil content in moisturizing compositions of the present disclosure isbetween 5% (v/v) and 15% (v/v).

In an embodiment, the percent shea butter content in moisturizingcompositions of the present disclosure is about 1% (v/v). In anembodiment, the percent shea butter content in moisturizing compositionsof the present disclosure is about 5% (v/v). In an embodiment, thepercent shea butter content in moisturizing compositions of the presentdisclosure is about 10% (v/v). In an embodiment, the percent shea buttercontent in moisturizing compositions of the present disclosure is about15% (v/v). In an embodiment, the percent shea butter content inmoisturizing compositions of the present disclosure is about 20% (v/v).In an embodiment, the percent shea butter content in moisturizingcompositions of the present disclosure is about 25% (v/v). In anembodiment, the percent shea butter content in moisturizing compositionsof the present disclosure is less than 25% (v/v). In an embodiment, thepercent shea butter content in moisturizing compositions of the presentdisclosure is less than 20% (v/v). In an embodiment, the percent sheabutter content in moisturizing compositions of the present disclosure isless than 15% (v/v). In an embodiment, the percent shea butter contentin moisturizing compositions of the present disclosure is less than 10%(v/v). In an embodiment, the percent shea butter content in moisturizingcompositions of the present disclosure is less than 5% (v/v). In anembodiment, the percent shea butter content in moisturizing compositionsof the present disclosure is less than 1% (v/v). In an embodiment, thepercent shea butter content in moisturizing compositions of the presentdisclosure is between 0% (v/v) and 25% (v/v). In an embodiment, thepercent shea butter content in moisturizing compositions of the presentdisclosure is between 0.1% (v/v) and 25% (v/v). In an embodiment, thepercent shea butter content in moisturizing compositions of the presentdisclosure is between 1% (v/v) and 20% (v/v). In an embodiment, thepercent shea butter content in moisturizing compositions of the presentdisclosure is between 5% (v/v) and 15% (v/v).

In an embodiment, the percent glycerin content in moisturizingcompositions of the present disclosure is about 0.5% (v/v). In anembodiment, the percent glycerin content in moisturizing compositions ofthe present disclosure is about 1% (v/v). In an embodiment, the percentglycerin content in moisturizing compositions of the present disclosureis about 5% (v/v). In an embodiment, the percent glycerin content inmoisturizing compositions of the present disclosure is about 10% (v/v).In an embodiment, the percent glycerin content in moisturizingcompositions of the present disclosure is about 15% (v/v). In anembodiment, the percent glycerin content in moisturizing compositions ofthe present disclosure is less than 15% (v/v). In an embodiment, thepercent glycerin content in moisturizing compositions of the presentdisclosure is less than 10% (v/v). In an embodiment, the percentglycerin content in moisturizing compositions of the present disclosureis less than 5% (v/v). In an embodiment, the percent glycerin content inmoisturizing compositions of the present disclosure is less than 1%(v/v). In an embodiment, the percent glycerin content in moisturizingcompositions of the present disclosure is between 0% (v/v) and 15%(v/v). In an embodiment, the percent glycerin content in moisturizingcompositions of the present disclosure is between 0.1% (v/v) and 10%(v/v). In an embodiment, the percent glycerin content in moisturizingcompositions of the present disclosure is between 1% (v/v) and 10%(v/v). In an embodiment, the percent glycerin content in moisturizingcompositions of the present disclosure is between 2% (v/v) and 8% (v/v).

In some embodiments, a moisturizing composition of the presentcomposition comprises an additive, for example, vitamin E, aspen bark,sodium anisate, oat flour, titanium dioxide, zinc oxide, honeysuckleblend, or a combination of two or more thereof. In one embodiment, amoisturizing composition can be used to deliver hydrophobic compounds.In one embodiment, a moisturizing composition can be used to deliverhydrophilic compounds. In one embodiment, a moisturizing composition canbe used to deliver both hydrophobic and hydrophilic compounds together.Additives may be included to address pigment reduction, sun protection,fragrance, anti-aging and wrinkles, skin lightening, skin softening,skin moisturizing, scar reduction, exfoliation, skin toning, and/or skinfirming. In an embodiment, the percent content of each additive, (e.g.,vitamin E, aspen bark, sodium anisate, oat flour, titanium dioxide, zincoxide, or honeysuckle blend) in moisturizing compositions of the presentdisclosure is about 0.1% (v/v) or (w/v). In an embodiment, the percentcontent of each additive, (e.g., vitamin E, aspen bark, sodium anisate,oat flour, titanium dioxide, zinc oxide, or honeysuckle blend) inmoisturizing compositions of the present disclosure is about 0.5% (v/v)or (w/v). In an embodiment, the percent content of each additive, (e.g.,vitamin E, aspen bark, sodium anisate, oat flour, titanium dioxide, zincoxide, or honeysuckle blend) in moisturizing compositions of the presentdisclosure is about 1% (v/v) or (w/v). In an embodiment, the percentcontent of each additive, (e.g., vitamin E, aspen bark, sodium anisate,oat flour, titanium dioxide, zinc oxide, or honeysuckle blend) inmoisturizing compositions of the present disclosure is about 1.5% (v/v)or (w/v). In an embodiment, the percent content of each additive, (e.g.,vitamin E, aspen bark, sodium anisate, oat flour, titanium dioxide, zincoxide, or honeysuckle blend) of the present disclosure is about 2% (v/v)or (w/v). In an embodiment, the percent content of each additive, (e.g.,vitamin E, aspen bark, sodium anisate, oat flour, titanium dioxide, zincoxide, or honeysuckle blend) in moisturizing compositions of the presentdisclosure is about 2.5% (v/v) or (w/v). In an embodiment, the percentcontent of each additive, (e.g., vitamin E, aspen bark, sodium anisate,oat flour, titanium dioxide, zinc oxide, or honeysuckle blend) inmoisturizing compositions of the present disclosure is about 3% (v/v) or(w/v). In an embodiment, the percent content of each additive, (e.g.,vitamin E, aspen bark, sodium anisate, oat flour, titanium dioxide, zincoxide, or honeysuckle blend) in moisturizing compositions of the presentdisclosure is about 3.5% (v/v) or (w/v). In an embodiment, the percentcontent of each additive, (e.g., vitamin E, aspen bark, sodium anisate,oat flour, titanium dioxide, zinc oxide, or honeysuckle blend) of thepresent disclosure is about 4% (v/v) or (w/v). In an embodiment, thepercent content of each additive, (e.g., vitamin E, aspen bark, sodiumanisate, oat flour, titanium dioxide, zinc oxide, or honeysuckle blend)in moisturizing compositions of the present disclosure is about 4.5%(v/v) or (w/v). In an embodiment, the percent content of each additive,(e.g., vitamin E, aspen bark, sodium anisate, oat flour, titaniumdioxide, zinc oxide, or honeysuckle blend) of the present disclosure isabout 5% (v/v) or (w/v). In an embodiment, the percent content of anadditive, (e.g., vitamin E, aspen bark, sodium anisate, oat flour,titanium dioxide, zinc oxide, or honeysuckle blend) in moisturizingcompositions of the present disclosure is less than 5% (v/v) or (w/v).In an embodiment, the percent content of an additive, (e.g., vitamin E,aspen bark, sodium anisate, oat flour, titanium dioxide, zinc oxide, orhoneysuckle blend) in moisturizing compositions of the presentdisclosure is less than 4.5% (v/v) or (w/v). In an embodiment, thepercent content of an additive, (e.g., vitamin E, aspen bark, sodiumanisate, oat flour, titanium dioxide, zinc oxide, or honeysuckle blend)in moisturizing compositions of the present disclosure is less than 4%(v/v) or (w/v). In an embodiment, the percent content of an additive,(e.g., vitamin E, aspen bark, sodium anisate, oat flour, titaniumdioxide, zinc oxide, or honeysuckle blend) in moisturizing compositionsof the present disclosure is less than 3.5% (v/v) or (w/v). In anembodiment, the percent content of an additive, (e.g., vitamin E, aspenbark, sodium anisate, oat flour, titanium dioxide, zinc oxide, orhoneysuckle blend) in moisturizing compositions of the presentdisclosure is less than 3% (v/v) or (w/v). In an embodiment, the percentcontent of an additive, (e.g., vitamin E, aspen bark, sodium anisate,oat flour, titanium dioxide, zinc oxide, or honeysuckle blend) inmoisturizing compositions of the present disclosure is less than 2.5%(v/v) or (w/v). In an embodiment, the percent content of an additive,(e.g., vitamin E, aspen bark, sodium anisate, oat flour, titaniumdioxide, zinc oxide, or honeysuckle blend) in moisturizing compositionsof the present disclosure is less than 2% (v/v) or (w/v). In anembodiment, the percent content of an additive, (e.g., vitamin E, aspenbark, sodium anisate, oat flour, titanium dioxide, zinc oxide, orhoneysuckle blend) in moisturizing compositions of the presentdisclosure is less than 1.5% (v/v) or (w/v). In an embodiment, thepercent content of an additive, (e.g., vitamin E, aspen bark, sodiumanisate, oat flour, titanium dioxide, zinc oxide, or honeysuckle blend)in moisturizing compositions of the present disclosure is less than 1%(v/v) or (w/v). In an embodiment, the percent content of an additive,(e.g., vitamin E, aspen bark, sodium anisate, oat flour, titaniumdioxide, zinc oxide, or honeysuckle blend) in moisturizing compositionsof the present disclosure is less than 0.5% (v/v) or (w/v). In anembodiment, the percent content of an additive, (e.g., vitamin E, aspenbark, sodium anisate, oat flour, titanium dioxide, zinc oxide, orhoneysuckle blend) in moisturizing compositions of the presentdisclosure is between 0% and 5% (v/v) or (w/v). In an embodiment, thepercent content of an additive, (e.g., vitamin E, aspen bark, sodiumanisate, oat flour, titanium dioxide, zinc oxide, or honeysuckle blend)in moisturizing compositions of the present disclosure is between 0.1%and 5% (v/v) or (w/v). In an embodiment, the percent content of anadditive, (e.g., vitamin E, aspen bark, sodium anisate, oat flour,titanium dioxide, zinc oxide, or honeysuckle blend) in moisturizingcompositions of the present disclosure is between 1% and 5% (v/v) or(w/v). In an embodiment, the percent content of an additive, (e.g.,vitamin E, aspen bark, sodium anisate, oat flour, titanium dioxide, zincoxide, or honeysuckle blend) in moisturizing compositions of the presentdisclosure is between 1% and 3% (v/v) or (w/v). In an embodiment, thepercent content of an additive, (e.g., vitamin E, aspen bark, sodiumanisate, oat flour, titanium dioxide, zinc oxide, or honeysuckle blend)in moisturizing compositions of the present disclosure is between 0.5%and 2% (v/v) or (w/v). In an embodiment, the percent content of anadditive, (e.g., vitamin E, aspen bark, sodium anisate, oat flour,titanium dioxide, zinc oxide, or honeysuckle blend) in moisturizingcompositions of the present disclosure is between 0.1% and 1% (v/v) or(w/v).

In some embodiments, a moisturizing composition of the presentcomposition comprises an agent for adjusting pH, for example, HCl, NaOH,or a combination thereof. In an embodiment, the percent content of eachpH adjusting agent, (e.g., HCl or NaOH) in moisturizing compositions ofthe present disclosure is about 0.05% (v/v). In an embodiment, thepercent content of each pH adjusting agent, (e.g., HCl or NaOH) inmoisturizing compositions of the present disclosure is about 0.1% (v/v).In an embodiment, the percent content of each pH adjusting agent, (e.g.,HCl or NaOH) in moisturizing compositions of the present disclosure isabout 0.15% (v/v). In an embodiment, the percent content of each pHadjusting agent, (e.g., HCl or NaOH) in moisturizing compositions of thepresent disclosure is about 0.2% (v/v). In an embodiment, the percentcontent of each pH adjusting agent, (e.g., HCl or NaOH) in moisturizingcompositions of the present disclosure is about 0.3% (v/v). In anembodiment, the percent content of each pH adjusting agent, (e.g., HClor NaOH) in moisturizing compositions of the present disclosure is about0.4% (v/v). In an embodiment, the percent content of each pH adjustingagent, (e.g., HCl or NaOH) in moisturizing compositions of the presentdisclosure is about 0.5% (v/v). In an embodiment, the percent content ofeach pH adjusting agent, (e.g., HCl or NaOH) in moisturizingcompositions of the present disclosure is about 0.6% (v/v). In anembodiment, the percent content of each pH adjusting agent, (e.g., HClor NaOH) in moisturizing compositions of the present disclosure is about0.7% (v/v). In an embodiment, the percent content of each pH adjustingagent, (e.g., HCl or NaOH) in moisturizing compositions of the presentdisclosure is about 0.8% (v/v). In an embodiment, the percent content ofeach pH adjusting agent, (e.g., HCl or NaOH) in moisturizingcompositions of the present disclosure is about 0.9% (v/v). In anembodiment, the percent content of each pH adjusting agent, (e.g., HClor NaOH) in moisturizing compositions of the present disclosure is about1% (v/v). In an embodiment, the percent content of each pH adjustingagent, (e.g., HCl or NaOH) in moisturizing compositions of the presentdisclosure is about 1.1% (v/v). In an embodiment, the percent content ofeach pH adjusting agent, (e.g., HCl or NaOH) in moisturizingcompositions of the present disclosure is about 1.2% (v/v). In anembodiment, the percent content of each pH adjusting agent, (e.g., HClor NaOH) in moisturizing compositions of the present disclosure is about1.3% (v/v). In an embodiment, the percent content of each pH adjustingagent, (e.g., HCl or NaOH) in moisturizing compositions of the presentdisclosure is about 1.4% (v/v). In an embodiment, the percent content ofeach pH adjusting agent, (e.g., HCl or NaOH) in moisturizingcompositions of the present disclosure is about 1.5% (v/v). In anembodiment, the percent content of each pH adjusting agent, (e.g., HClor NaOH) in moisturizing compositions of the present disclosure is lessthan 1.5% (v/v). In an embodiment, the percent content of each pHadjusting agent, (e.g., HCl (e.g. 2M HCl) or NaOH (e.g. 5N NaOH)) inmoisturizing compositions of the present disclosure is less than 1.4%(v/v). In an embodiment, the percent content of each pH adjusting agent,(e.g., HCl or NaOH) in moisturizing compositions of the presentdisclosure is less than 1.3% (v/v). In an embodiment, the percentcontent of each pH adjusting agent, (e.g., HCl or NaOH) in moisturizingcompositions of the present disclosure is less than 1.2% (v/v). In anembodiment, the percent content of each pH adjusting agent, (e.g., HClor NaOH) in moisturizing compositions of the present disclosure is lessthan 1.1% (v/v). In an embodiment, the percent content of each pHadjusting agent, (e.g., HCl or NaOH) in moisturizing compositions of thepresent disclosure is less than 1% (v/v). In an embodiment, the percentcontent of each pH adjusting agent, (e.g., HCl or NaOH) in moisturizingcompositions of the present disclosure is less than 0.9% (v/v). In anembodiment, the percent content of each pH adjusting agent, (e.g., HClor NaOH) in moisturizing compositions of the present disclosure is lessthan 0.8% (v/v). In an embodiment, the percent content of each pHadjusting agent, (e.g., HCl or NaOH) in moisturizing compositions of thepresent disclosure is less than 0.7% (v/v). In an embodiment, thepercent content of each pH adjusting agent, (e.g., HCl or NaOH) inmoisturizing compositions of the present disclosure is less than 0.6%(v/v). In an embodiment, the percent content of each pH adjusting agent,(e.g., HCl or NaOH) in moisturizing compositions of the presentdisclosure is less than 0.5% (v/v). In an embodiment, the percentcontent of each pH adjusting agent, (e.g., HCl or NaOH) in moisturizingcompositions of the present disclosure is less than 0.4% (v/v). In anembodiment, the percent content of each pH adjusting agent, (e.g., HClor NaOH) in moisturizing compositions of the present disclosure is lessthan 0.3% (v/v). In an embodiment, the percent content of each pHadjusting agent, (e.g., HCl or NaOH) in moisturizing compositions of thepresent disclosure is less than 0.2% (v/v). In an embodiment, thepercent content of each pH adjusting agent, (e.g., HCl or NaOH) inmoisturizing compositions of the present disclosure is less than 0.1%(v/v). In an embodiment, the percent content of each pH adjusting agent,(e.g., HCl or NaOH) in moisturizing compositions of the presentdisclosure is between 0.1% and 1.5% (v/v). In an embodiment, the percentcontent of each pH adjusting agent, (e.g., HCl or NaOH) in moisturizingcompositions of the present disclosure is between 0.5% and 1.5% (v/v).In an embodiment, the percent content of each pH adjusting agent, (e.g.,HCl or NaOH) in moisturizing compositions of the present disclosure isbetween 1% and 1.5% (v/v). In an embodiment, the percent content of eachpH adjusting agent, (e.g., HCl or NaOH) in moisturizing compositions ofthe present disclosure is between 0.1% and 0.5% (v/v).

According to aspects illustrated herein, there is disclosed a method forpreparing a moisturizing composition comprising pure silk fibroin-basedprotein fragments disclosed herein. Water (e.g. RO/DI) is poured into abeaker or KitchenAid bowl. Hyaluronic acid powder is added to the water.The solution is mixed vigorously at a power of 6-10 (KitchenAid) or300-700 rpm (lab mixer) until the hyaluronic acid is fully dissolved(about 1-3 hours). A solution of pure silk fibroin based proteinfragments is added to the hyaluronic acid solution and mixed gently at apower of 2 (KitchenAid) or 50-80 rpm (lab mixer) until silk andhyaluronic acid solution are homogenous. The silk/hyaluronic acidsolution is stored in a refrigerator overnight. The solution may betransferred to another container. Jojoba oil, rosehip oil, vitamin E,and 5N NaOH are mixed. The hyaluronic acid/silk solution is mixed at apower of 4-10 (KitchenAid) or 300-700 rpm (lab mixer); the jojoba oil,rosehip oil, vitamin E, 5N NaOH mixture are added to the hyaluronicacid/silk solution. The solution is mixed until a white, lotion-likehomogeneous mixture is formed. Continue to mix for at least 10 minutes.2M HCl is added and the solution is mixed at a power of 4-10(KitchenAid) 300-700 rpm (lab mixer) for at least 15 minutes. Aspen barkis added and the solution is mixed at a power of 4-10 (KitchenAid)300-700 rpm (lab mixer) for at least 15 minutes. Sodium anisate is addedand the solution is mixed at a power of 4-10 (KitchenAid) 300-700 rpm(lab mixer) for at least 15 minutes to form the final moisturizercomposition. In some embodiments, the foregoing method may be used forthe preparation of a 1 liter batch moisturizer composition.

In some embodiments, a composition of the present disclosure can furtherinclude skin penetration enhancers, including, but not limited to,sulfoxides (such as dimethylsulfoxide), pyrrolidones (such as2-pyrrolidone), alcohols (such as ethanol or decanal), azones (such aslaurocapram and 1-dodecylazacycloheptan-2-one), surfactants (includingalkyl carboxylates and their corresponding acids such as oleic acid,fluoroalkylcarboxylates and their corresponding acids, alkyl sulfates,alky! ether sulfates, docusates such as dioctyl sodium sulfosuccinate,alkyl benzene sulfonates, alkyl ether phosphates, and alkyl aryl etherphosphates), glycols (such as propylene glycol), terpenes (such aslimonene, p-cymene, geraniol, farnesol, eugenol, menthol, terpineol,carveol, carvone, fenchone, and verbenone), and dimethyl isosorbide.

In an embodiment, a solution of the present disclosure is contacted witha therapeutic agent and/or a molecule prior to forming the article. Inan embodiment, molecules include, but are not limited to, antioxidantsand enzymes. In an embodiment, molecules include, but are not limited toSelenium, Ubiquinone derivatives, Thiol-based antioxidants,Saccharide-containing antioxidants, Polyphenols, Botanical extracts,Caffeic acid, Apigenin, Pycnogenol, Resveratrol, Folic acid, Vitaminb12, Vitamin b6. Vitamin b3, Vitamin E, Vitamin C and derivativesthereof, Vitamin D, Vitamin A, Astaxathm, Lutein, Lycopene, Essentialfatty acids (omegas 3 and 6), Iron, Zinc, magnesium, Flavonoids (soy,Cureumin, Silymarm, Pycnongeol), Growth factors, aloe, hyaluronic acid,extracellular matrix proteins, cells, nucleic acids, biomarkers,biological reagents, zinc oxide, benzoyl peroxide, retnoids, titanium,allergens in a known dose (for sensitization treatment), essential oilsincluding, but not limited to, lemongrass or rosemary oil, andfragrances. Therapeutic agents include, but are not limited to, smallmolecules, drugs, proteins, peptides and nucleic acids. In anembodiment, a silk moisturizing composition of the present disclosureincludes a molecule that is a vitamin, such as vitamin C, vitamin A andvitamin E. In an embodiment, a solution of the present disclosure iscontacted with an allergen of known quantity prior to forming thearticle. Allergens include but are not limited to milk, eggs, peanuts,tree nuts, fish, shellfish, soy and wheat. Known doses of allergenloaded within a silk article can be released at a known rate forcontrolled exposure allergy study, tests and sensitization treatment.

In an embodiment, a moisturizer composition further includes an amountof vitamin C, Vitamin B, Vitamin A, or a derivative thereof, of about 50wt. %, about 45 wt. %, about 40 wt. %, about 35 wt. %, about 30 wt. %,about 25 wt. %, about 20 wt. %, about 19.75 wt. %, about 19.50 wt. %,about 19.25 wt. %, about 19 wt. %, about 18.75 wt. %, about 18.50 wt. %,about 18.25 wt. %, about 18 wt. %, about 17.75 wt. %, about 17.50 wt. %,about 17.25 wt. %, about 17 wt. %, about 16.75 wt. %, about 16.50 wt. %,about 16.25 wt. % about 16 wt. %, about 15.75 wt. %, about 15.50 wt. %,about 15.25 wt. %, about 15 wt. %, about 14.75 wt. %, about 14.50 wt. %,about 14.25 wt. %, about 14 wt. %, about 13.75 wt. %, about 13.50 wt. %,about 13.25 wt. %, about 13 wt. %, about 12.75 wt. %, about 12.50 wt. %,about 12.25 wt. %, about 12 wt. %, about 11.75 wt. %, about 11.50 wt. %,about 11.25 wt. %, about 11 wt. %, about 10.75 wt. %, about 10.50 wt. %,about 10.25 wt. %, about 10 wt. %, about 9.75 wt. %, about 9.50 wt. %,about 9.25 wt. %, about 9 wt. %, about 8.75 wt. %, about 8.50 wt. %,about 8.25 wt. %, about 8 wt. %, about 7.75 wt. %, about 7.50 wt. %,about 7.25 wt. %, about 7 wt. %, about 6.75 wt. %, about 6.50 wt. %,about 6.25 wt. %, about 6 wt. %, about 5.75 wt. %, about 5.50 wt. %,about 5.25 wt. %, about 5 wt. %, about 4.75 wt. %, about 4.50 wt. %,about 4.25 wt. %, about 4 wt. %, about 3.75 wt. %, about 3.50 wt. %,about 3.25 wt. %, about 3 wt. %, about 2.75 wt. %, about 2.50 wt. %,about 2.25 wt. %, about 2 wt. %, about 1.75 wt. %, about 1.50 wt. %,about 1.25 wt. %, about 1 wt. %, about 0.5 wt. %, about 0.4 wt. %, about0.3 wt. %, about 0.2 wt. %, about 0.1 wt. %, about 0.09 wt. %, about0.08 wt. %, about 0.07 wt. %, about 0.06 wt. %, about 0.05 wt. %, about0.04 wt. %, about 0.03 wt. %, about 0.02 wt. %, about 0.01 wt. %, about0.009 wt. %, about 0.008 wt. %, about 0.007 wt. %, about 0.006 wt. %,about 0.005 wt. %, about 0.004 wt. %, about 0.003 wt. %, about 0.002 wt.%, or about 0.001 wt. %.

In an embodiment, a moisturizer composition further includes an amountof vitamin C, Vitamin B, Vitamin A, or a derivative thereof, of betweenabout 1 wt. % to about 50 wt. %, between about 2 wt. % to about 40 wt.%, between about 3 wt. % to about 30 wt. %, between about 4 wt. % toabout 20 wt. %, between about 5 wt. % to about 15 wt. %, between about 6wt. % to about 10 wt. %, between about 7 wt. % to about 9 wt. %, betweenabout 10 wt. % to about 50 wt. %, between about 15 wt. % to about 45 wt.%, between about 20 wt. % to about 40 wt. %, between about 25 wt. % toabout 35 wt. %, or between about 25 wt. % to about 30 wt. %.

In an embodiment, a moisturizer composition further includes an amountof vitamin C, Vitamin B, Vitamin A, or a derivative thereof, of betweenabout 0.001 wt. % to about 5 wt. %, between about 5 wt. % to about 10wt. %, between about 10 wt. % to about 15 wt. %, between about 15 wt. %to about 20 wt. %, between about 20 wt. % to about 25 wt. %, betweenabout 25 wt. % to about 30 wt. %, between about 30 wt. % to about 35 wt.%, between about 35 wt. % to about 40 wt. %, between about 40 wt. % toabout 45 wt. %, or between about 45 wt. % to about 50 wt. %.

In an embodiment, a moisturizer composition further includes an amountof vitamin C, Vitamin B, Vitamin A, or a derivative thereof, of betweenabout 0.001 wt. % to about 1 wt. %, between about 1 wt. % to about 2 wt.%, between about 2 wt. % to about 3 wt. %, between about 3 wt. % toabout 4 wt. %, between about 4 wt. % to about 5 wt. %, between about 5wt. % to about 6 wt. %, between about 6 wt. % to about 7 wt. %, betweenabout 7 wt. % to about 8 wt. %, between about 8 wt. % to about 9 wt. %,between about 9 wt. % to about 10 wt. %, between about 10 wt. % to about11 wt. %, between about 11 wt. % to about 12 wt. %, between about 12 wt.% to about 13 wt. %, between about 13 wt. % to about 14 wt. %, betweenabout 14 wt. % to about 15 wt. %, between about 15 wt. % to about 16 wt.%, between about 16 wt. % to about 17 wt. %, between about 17 wt. % toabout 18 wt. %, between about 18 wt. % to about 19 wt. %, between about19 wt. % to about 20 wt. %, between about 20 wt. % to about 21 wt. %,between about 21 wt. % to about 22 wt. %, between about 22 wt. % toabout 23 wt. %, between about 23 wt. % to about 24 wt. %, between about24 wt. % to about 25 wt. %, between about 25 wt. % to about 26 wt. %,between about 26 wt. % to about 27 wt. %, between about 27 wt. % toabout 28 wt. %, between about 28 wt. % to about 29 wt. %, between about29 wt. % to about 30 wt. %, between about 30 wt. % to about 31 wt. %,between about 31 wt. % to about 32 wt. %, between about 32 wt. % toabout 33 wt. %, between about 33 wt. % to about 34 wt. %, between about34 wt. % to about 35 wt. %, between about 35 wt. % to about 36 wt. %,between about 36 wt. % to about 37 wt. %, between about 37 wt. % toabout 38 wt. %, between about 38 wt. % to about 39 wt. %, between about39 wt. % to about 40 wt. %, between about 40 wt. % to about 41 wt. %,between about 41 wt. % to about 42 wt. %, between about 42 wt. % toabout 43 wt. %, between about 43 wt. % to about 44 wt. %, between about44 wt. % to about 45 wt. %, between about 45 wt. % to about 46 wt. %,between about 46 wt. % to about 47 wt. %, between about 47 wt. % toabout 48 wt. %, between about 48 wt. % to about 49 wt. %, or betweenabout 49 wt. % to about 50 wt. %.

In an embodiment, a moisturizer composition further includes an amountof vitamin C, Vitamin B, Vitamin A, or a derivative thereof, of 50 wt.%, 45 wt. %, 40 wt. %, 35 wt. %, 30 wt. %, 25 wt. %, 20 wt. %, 19.75 wt.%, 19.50 wt. %, 19.25 wt. %, 19 wt. %, 18.75 wt. %, 18.50 wt. %, 18.25wt. %, 18 wt. %, 17.75 wt. %, 17.50 wt. %, 17.25 wt. %, 17 wt. %, 16.75wt. %, 16.50 wt. %, 16.25 wt. % 16 wt. %, 15.75 wt. %, 15.50 wt. %,15.25 wt. %, 15 wt. %, 14.75 wt. %, 14.50 wt. %, 14.25 wt. %, 14 wt. %,13.75 wt. %, 13.50 wt. %, 13.25 wt. %, 13 wt. %, 12.75 wt. %, 12.50 wt.%, 12.25 wt. %, 12 wt. %, 11.75 wt. %, 11.50 wt. %, 11.25 wt. %, 11 wt.%, 10.75 wt. %, 10.50 wt. %, 10.25 wt. %, 10 wt. %, 9.75 wt. %, 9.50 wt.%, 9.25 wt. %, 9 wt. %, 8.75 wt. %, 8.50 wt. %, 8.25 wt. %, 8 wt. %,7.75 wt. %, 7.50 wt. %, 7.25 wt. %, 7 wt. %, 6.75 wt. %, 6.50 wt. %,6.25 wt. %, 6 wt. %, 5.75 wt. %, 5.50 wt. %, 5.25 wt. %, 5 wt. %, 4.75wt. %, 4.50 wt. %, 4.25 wt. %, 4 wt. %, 3.75 wt. %, 3.50 wt. %, 3.25 wt.%, 3 wt. %, 2.75 wt. %, 2.50 wt. %, 2.25 wt. %, 2 wt. %, 1.75 wt. %,1.50 wt. %, 1.25 wt. %, 1 wt. %, 0.5 wt. %, 0.4 wt. %, 0.3 wt. %, 0.2wt. %, 0.1 wt. %, 0.09 wt. %, 0.08 wt. %, 0.07 wt. %, 0.06 wt. %, 0.05wt. %, 0.04 wt. %, 0.03 wt. %, 0.02 wt. %, 0.01 wt. %, 0.009 wt. %,0.008 wt. %, 0.007 wt. %, 0.006 wt. %, 0.005 wt. %, 0.004 wt. %, 0.003wt. %, 0.002 wt. %, or 0.001 wt. %.

In an embodiment, a moisturizer composition further includes an amountof vitamin C, Vitamin B, Vitamin A, or a derivative thereof, of between1 wt. % to 50 wt. %, between 2 wt. % to 40 wt. %, between 3 wt. % to 30wt. %, between 4 wt. % to 20 wt. %, between 5 wt. % to 15 wt. %, between6 wt. % to 10 wt. %, between 7 wt. % to 9 wt. %, between 10 wt. % to 50wt. %, between 15 wt. % to 45 wt. %, between 20 wt. % to 40 wt. %,between 25 wt. % to 35 wt. %, or between 30 wt. % to 35 wt. %.

In an embodiment, a moisturizer composition further includes an amountof vitamin C, Vitamin B, Vitamin A, or a derivative thereof, of between0.001 wt. % to 5 wt. %, between 5 wt. % to 10 wt. %, between 10 wt. % to15 wt. %, between 15 wt. % to 20 wt. %, between 20 wt. % to 25 wt. %,between 25 wt. % to 30 wt. %, between 30 wt. % to 35 wt. %, between 35wt. % to 40 wt. %, between 40 wt. % to 45 wt. %, or between 45 wt. % to50 wt. %.

In an embodiment, a moisturizer composition further includes an amountof vitamin C, Vitamin B, Vitamin A, or a derivative thereof, of between0.001 wt. % to 1 wt. %, between 1 wt. % to 2 wt. %, between 2 wt. % to 3wt. %, between 3 wt. % to 4 wt. %, between 4 wt. % to 5 wt. %, between 5wt. % to 6 wt. %, between 6 wt. % to 7 wt. %, between 7 wt. % to 8 wt.%, between 8 wt. % to 9 wt. %, between 9 wt. % to 10 wt. %, between 10wt. % to 11 wt. %, between 11 wt. % to 12 wt. %, between 12 wt. % to 13wt. %, between 13 wt. % to 14 wt. %, between 14 wt. % to 15 wt. %,between 15 wt. % to 16 wt. %, between 16 wt. % to 17 wt. %, between 17wt. % to 18 wt. %, between 18 wt. % to 19 wt. %, between 19 wt. % to 20wt. %, between 20 wt. % to 21 wt. %, between 21 wt. % to 22 wt. %,between 22 wt. % to 23 wt. %, between 23 wt. % to 24 wt. %, between 24wt. % to 25 wt. %, between 25 wt. % to 26 wt. %, between 26 wt. % to 27wt. %, between 27 wt. % to 28 wt. %, between 28 wt. % to 29 wt. %,between 29 wt. % to 30 wt. %, between 30 wt. % to 31 wt. %, between 31wt. % to 32 wt. %, between 32 wt. % to 33 wt. %, between 33 wt. % to 34wt. %, between 34 wt. % to 35 wt. %, between 35 wt. % to 36 wt. %,between 36 wt. % to 37 wt. %, between 37 wt. % to 38 wt. %, between 38wt. % to 39 wt. %, between 39 wt. % to 40 wt. %, between 40 wt. % to 41wt. %, between 41 wt. % to 42 wt. %, between 42 wt. % to 43 wt. %,between 43 wt. % to 44 wt. %, between 44 wt. % to 45 wt. %, between 45wt. % to 46 wt. %, between 46 wt. % to 47 wt. %, between 47 wt. % to 48wt. %, between 48 wt. % to 49 wt. %, or between 49 wt. % to 50 wt. %.

In an embodiment, a moisturizer composition further includes an amountof vitamin C, Vitamin B, Vitamin A, or a derivative thereof, of lessthan 50 wt. %, less than 40 wt. %, less than 30 wt. %, less than 20 wt.%, less than 19.75 wt. %, less than 19.50 wt. %, less than 19.25 wt. %,less than 19 wt. %, less than 18.75 wt. %, less than 18.50 wt. %, lessthan 18.25 wt. %, less than 18 wt. %, less than 17.75 wt. %, less than17.50 wt. %, less than 17.25 wt. %, less than 17 wt. %, less than 16.75wt. %, less than 16.50 wt. %, less than 16.25 wt. % less than 16 wt. %,less than 15.75 wt. %, less than 15.50 wt. %, less than 15.25 wt. %,less than 15 wt. %, less than 14.75 wt. %, less than 14.50 wt. %, lessthan 14.25 wt. %, less than 14 wt. %, less than 13.75 wt. %, less than13.50 wt. %, less than 13.25 wt. %, less than 13 wt. %, less than 12.75wt. %, less than 12.50 wt. %, less than 12.25 wt. %, less than 12 wt. %,less than 11.75 wt. %, less than 11.50 wt. %, less than 11.25 wt. %,less than 11 wt. %, less than 10.75 wt. %, less than 10.50 wt. %, lessthan 10.25 wt. %, less than 10 wt. %, less than 9.75 wt. %, less than9.50 wt. %, less than 9.25 wt. %, less than 9 wt. %, less than 8.75 wt.%, less than 8.50 wt. %, less than 8.25 wt. %, less than 8 wt. %, lessthan 7.75 wt. %, less than 7.50 wt. %, less than 7.25 wt. %, less than 7wt. %, less than 6.75 wt. %, less than 6.50 wt. %, less than 6.25 wt. %,less than 6 wt. %, less than 5.75 wt. %, less than 5.50 wt. %, less than5.25 wt. %, less than 5 wt. %, less than 4.75 wt. %, less than 4.50 wt.%, less than 4.25 wt. %, less than 4 wt. %, less than 3.75 wt. %, lessthan 3.50 wt. %, less than 3.25 wt. %, less than 3 wt. %, less than 2.75wt. %, less than 2.50 wt. %, less than 2.25 wt. %, less than 2 wt. %,less than 1.75 wt. %, less than 1.50 wt. %, less than 1.25 wt. %, lessthan 1 wt. %, less than 0.5 wt. %, less than 0.4 wt. %, less than 0.3wt. %, less than 0.2 wt. %, less than 0.1 wt. %, less than 0.09 wt. %,less than 0.08 wt. %, less than 0.07 wt. %, less than 0.06 wt. %, lessthan 0.05 wt. %, less than 0.04 wt. %, less than 0.03 wt. %, less than0.02 wt. %, less than 0.01 wt. %, less than 0.009 wt. %, less than 0.008wt. %, less than 0.007 wt. %, less than 0.006 wt. %, less than 0.005 wt.%, less than 0.004 wt. %, less than 0.003 wt. %, less than 0.002 wt. %,or less than 0.001 wt. %.

In an embodiment, the moisturizer composition further includes an amountof vitamin C, Vitamin B, Vitamin A, or a derivative thereof, of greaterthan 45 wt. %, greater than 40 wt. %, greater than 30 wt. %, greaterthan 20 wt. %, greater than 19.75 wt. %, greater than 19.50 wt. %,greater than 19.25 wt. %, greater than 19 wt. %, greater than 18.75 wt.%, greater than 18.50 wt. %, greater than 18.25 wt. %, greater than 18wt. %, greater than 17.75 wt. %, greater than 17.50 wt. %, greater than17.25 wt. %, greater than 17 wt. %, greater than 16.75 wt. %, greaterthan 16.50 wt. %, greater than 16.25 wt. % greater than 16 wt. %,greater than 15.75 wt. %, greater than 15.50 wt. %, greater than 15.25wt. %, greater than 15 wt. %, greater than 14.75 wt. %, greater than14.50 wt. %, greater than 14.25 wt. %, greater than 14 wt. %, greaterthan 13.75 wt. %, greater than 13.50 wt. %, greater than 13.25 wt. %,greater than 13 wt. %, greater than 12.75 wt. %, greater than 12.50 wt.%, greater than 12.25 wt. %, greater than 12 wt. %, greater than 11.75wt. %, greater than 11.50 wt. %, greater than 11.25 wt. %, greater than11 wt. %, greater than 10.75 wt. %, greater than 10.50 wt. %, greaterthan 10.25 wt. %, greater than 10 wt. %, greater than 9.75 wt. %,greater than 9.50 wt. %, greater than 9.25 wt. %, greater than 9 wt. %,greater than 8.75 wt. %, greater than 8.50 wt. %, greater than 8.25 wt.%, greater than 8 wt. %, greater than 7.75 wt. %, greater than 7.50 wt.%, greater than 7.25 wt. %, greater than 7 wt. %, greater than 6.75 wt.%, greater than 6.50 wt. %, greater than 6.25 wt. %, greater than 6 wt.%, greater than 5.75 wt. %, greater than 5.50 wt. %, greater than 5.25wt. %, greater than 5 wt. %, greater than 4.75 wt. %, greater than 4.50wt. %, greater than 4.25 wt. %, greater than 4 wt. %, greater than 3.75wt. %, greater than 3.50 wt. %, greater than 3.25 wt. %, greater than 3wt. %, greater than 2.75 wt. %, greater than 2.50 wt. %, greater than2.25 wt. %, greater than 2 wt. %, greater than 1.75 wt. %, greater than1.50 wt. %, greater than 1.25 wt. %, greater than 1 wt. %, greater than0.5 wt. %, greater than 0.4 wt. %, greater than 0.3 wt. %, greater than0.2 wt. %, greater than 0.1 wt. %, greater than 0.09 wt. %, greater than0.08 wt. %, greater than 0.07 wt. %, greater than 0.06 wt. %, greaterthan 0.05 wt. %, greater than 0.04 wt. %, greater than 0.03 wt. %,greater than 0.02 wt. %, greater than 0.01 wt. %, greater than 0.009 wt.%, greater than 0.008 wt. %, greater than 0.007 wt. %, greater than0.006 wt. %, greater than 0.005 wt. %, greater than 0.004 wt. %, greaterthan 0.003 wt. %, greater than 0.002 wt. %, or greater than 0.001 wt. %.

In an embodiment, a moisturizer composition further includes an amountof vitamin E, or a derivative thereof, of about 50 wt. %, about 45 wt.%, about 40 wt. %, about 35 wt. %, about 30 wt. %, about 25 wt. %, about20 wt. %, about 19.75 wt. %, about 19.50 wt. %, about 19.25 wt. %, about19 wt. %, about 18.75 wt. %, about 18.50 wt. %, about 18.25 wt. %, about18 wt. %, about 17.75 wt. %, about 17.50 wt. %, about 17.25 wt. %, about17 wt. %, about 16.75 wt. %, about 16.50 wt. %, about 16.25 wt. % about16 wt. %, about 15.75 wt. %, about 15.50 wt. %, about 15.25 wt. %, about15 wt. %, about 14.75 wt. %, about 14.50 wt. %, about 14.25 wt. %, about14 wt. %, about 13.75 wt. %, about 13.50 wt. %, about 13.25 wt. %, about13 wt. %, about 12.75 wt. %, about 12.50 wt. %, about 12.25 wt. %, about12 wt. %, about 11.75 wt. %, about 11.50 wt. %, about 11.25 wt. %, about11 wt. %, about 10.75 wt. %, about 10.50 wt. %, about 10.25 wt. %, about10 wt. %, about 9.75 wt. %, about 9.50 wt. %, about 9.25 wt. %, about 9wt. %, about 8.75 wt. %, about 8.50 wt. %, about 8.25 wt. %, about 8 wt.%, about 7.75 wt. %, about 7.50 wt. %, about 7.25 wt. %, about 7 wt. %,about 6.75 wt. %, about 6.50 wt. %, about 6.25 wt. %, about 6 wt. %,about 5.75 wt. %, about 5.50 wt. %, about 5.25 wt. %, about 5 wt. %,about 4.75 wt. %, about 4.50 wt. %, about 4.25 wt. %, about 4 wt. %,about 3.75 wt. %, about 3.50 wt. %, about 3.25 wt. %, about 3 wt. %,about 2.75 wt. %, about 2.50 wt. %, about 2.25 wt. %, about 2 wt. %,about 1.75 wt. %, about 1.50 wt. %, about 1.25 wt. %, about 1 wt. %,about 0.5 wt. %, about 0.4 wt. %, about 0.3 wt. %, about 0.2 wt. %,about 0.1 wt. %, about 0.09 wt. %, about 0.08 wt. %, about 0.07 wt. %,about 0.06 wt. %, about 0.05 wt. %, about 0.04 wt. %, about 0.03 wt. %,about 0.02 wt. %, about 0.01 wt. %, about 0.009 wt. %, about 0.008 wt.%, about 0.007 wt. %, about 0.006 wt. %, about 0.005 wt. %, about 0.004wt. %, about 0.003 wt. %, about 0.002 wt. %, or about 0.001 wt. %.

In an embodiment, a moisturizer composition further includes an amountof vitamin E, or a derivative thereof, of between about 1 wt. % to about50 wt. %, between about 2 wt. % to about 40 wt. %, between about 3 wt. %to about 30 wt. %, between about 4 wt. % to about 20 wt. %, betweenabout 5 wt. % to about 15 wt. %, between about 6 wt. % to about 10 wt.%, between about 7 wt. % to about 9 wt. %, between about 10 wt. % toabout 50 wt. %, between about 15 wt. % to about 45 wt. %, between about20 wt. % to about 40 wt. %, between about 25 wt. % to about 35 wt. %, orbetween about 25 wt. % to about 30 wt. %.

In an embodiment, a moisturizer composition further includes an amountof vitamin E, or a derivative thereof, of between about 0.001 wt. % toabout 5 wt. %, between about 5 wt. % to about 10 wt. %, between about 10wt. % to about 15 wt. %, between about 15 wt. % to about 20 wt. %,between about 20 wt. % to about 25 wt. %, between about 25 wt. % toabout 30 wt. %, between about 30 wt. % to about 35 wt. %, between about35 wt. % to about 40 wt. %, between about 40 wt. % to about 45 wt. %, orbetween about 45 wt. % to about 50 wt. %.

In an embodiment, a moisturizer composition further includes an amountof vitamin E, or a derivative thereof, of between about 0.001 wt. % toabout 1 wt. %, between about 1 wt. % to about 2 wt. %, between about 2wt. % to about 3 wt. %, between about 3 wt. % to about 4 wt. %, betweenabout 4 wt. % to about 5 wt. %, between about 5 wt. % to about 6 wt. %,between about 6 wt. % to about 7 wt. %, between about 7 wt. % to about 8wt. %, between about 8 wt. % to about 9 wt. %, between about 9 wt. % toabout 10 wt. %, between about 10 wt. % to about 11 wt. %, between about11 wt. % to about 12 wt. %, between about 12 wt. % to about 13 wt. %,between about 13 wt. % to about 14 wt. %, between about 14 wt. % toabout 15 wt. %, between about 15 wt. % to about 16 wt. %, between about16 wt. % to about 17 wt. %, between about 17 wt. % to about 18 wt. %,between about 18 wt. % to about 19 wt. %, between about 19 wt. % toabout 20 wt. %, between about 20 wt. % to about 21 wt. %, between about21 wt. % to about 22 wt. %, between about 22 wt. % to about 23 wt. %,between about 23 wt. % to about 24 wt. %, between about 24 wt. % toabout 25 wt. %, between about 25 wt. % to about 26 wt. %, between about26 wt. % to about 27 wt. %, between about 27 wt. % to about 28 wt. %,between about 28 wt. % to about 29 wt. %, between about 29 wt. to about30 wt. %, between about 30 wt. % to about 31 wt. %, between about 31 wt.% to about 32 wt. %, between about 32 wt. % to about 33 wt. %, betweenabout 33 wt. % to about 34 wt. %, between about 34 wt. % to about 35 wt.%, between about 35 wt. % to about 36 wt. %, between about 36 wt. % toabout 37 wt. %, between about 37 wt. % to about 38 wt. %, between about38 wt. % to about 39 wt. %, between about 39 wt. % to about 40 wt. %,between about 40 wt. % to about 41 wt. %, between about 41 wt. % toabout 42 wt. %, between about 42 wt. % to about 43 wt. %, between about43 wt. % to about 44 wt. %, between about 44 wt. % to about 45 wt. %,between about 45 wt. % to about 46 wt. %, between about 46 wt. % toabout 47 wt. %, between about 47 wt. % to about 48 wt. %, between about48 wt. % to about 49 wt. %, or between about 49 wt. % to about 50 wt. %.

In an embodiment, a moisturizer composition further includes an amountof vitamin E, or a derivative thereof, of 50 wt. %, 45 wt. %, 40 wt. %,35 wt. %, 30 wt. %, 25 wt. %, 20 wt. %, 19.75 wt. %, 19.50 wt. %, 19.25wt. %, 19 wt. %, 18.75 wt. %, 18.50 wt. %, 18.25 wt. %, 18 wt. %, 17.75wt. %, 17.50 wt. %, 17.25 wt. %, 17 wt. %, 16.75 wt. %, 16.50 wt. %,16.25 wt. % 16 wt. %, 15.75 wt. %, 15.50 wt. %, 15.25 wt. %, 15 wt. %,14.75 wt. %, 14.50 wt. %, 14.25 wt. %, 14 wt. %, 13.75 wt. %, 13.50 wt.%, 13.25 wt. %, 13 wt. %, 12.75 wt. %, 12.50 wt. %, 12.25 wt. %, 12 wt.%, 11.75 wt. %, 11.50 wt. %, 11.25 wt. %, 11 wt. %, 10.75 wt. %, 10.50wt. %, 10.25 wt. %, 10 wt. %, 9.75 wt. %, 9.50 wt. %, 9.25 wt. %, 9 wt.%, 8.75 wt. %, 8.50 wt. %, 8.25 wt. %, 8 wt. %, 7.75 wt. %, 7.50 wt. %,7.25 wt. %, 7 wt. %, 6.75 wt. %, 6.50 wt. %, 6.25 wt. %, 6 wt. %, 5.75wt. %, 5.50 wt. %, 5.25 wt. %, 5 wt. %, 4.75 wt. %, 4.50 wt. %, 4.25 wt.%, 4 wt. %, 3.75 wt. %, 3.50 wt. %, 3.25 wt. %, 3 wt. %, 2.75 wt. %,2.50 wt. %, 2.25 wt. %, 2 wt. %, 1.75 wt. %, 1.50 wt. %, 1.25 wt. %, 1wt. %, 0.5 wt. %, 0.4 wt. %, 0.3 wt. %, 0.2 wt. %, 0.1 wt. %, 0.09 wt.%, 0.08 wt. %, 0.07 wt. %, 0.06 wt. %, 0.05 wt. %, 0.04 wt. %, 0.03 wt.%, 0.02 wt. %, 0.01 wt. %, 0.009 wt. %, 0.008 wt. %, 0.007 wt. %, 0.006wt. %, 0.005 wt. %, 0.004 wt. %, 0.003 wt. %, 0.002 wt. %, or 0.001 wt.%.

In an embodiment, a moisturizer composition further includes an amountof vitamin E, or a derivative thereof, of between 1 wt. % to 50 wt. %,between 2 wt. % to 40 wt. %, between 3 wt. % to 30 wt. %, between 4 wt.% to 20 wt. %, between 5 wt. % to 15 wt. %, between 6 wt. % to 10 wt. %,between 7 wt. % to 9 wt. %, between 10 wt. % to 50 wt. %, between 15 wt.% to 45 wt. %, between 20 wt. % to 40 wt. %, between 25 wt. % to 35 wt.%, or between 30 wt. % to 35 wt. %.

In an embodiment, a moisturizer composition further includes an amountof vitamin E, or a derivative thereof, of between 0.001 wt. % to 5 wt.%, between 5 wt. % to 10 wt. %, between 10 wt. % to 15 wt. %, between 15wt. % to 20 wt. %, between 20 wt. % to 25 wt. %, between 25 wt. % to 30wt. %, between 30 wt. % to 35 wt. %, between 35 wt. % to 40 wt. %,between 40 wt. % to 45 wt. %, or between 45 wt. % to 50 wt. %.

In an embodiment, a moisturizer composition further includes an amountof vitamin E, or a derivative thereof, of between 0.001 wt. % to 1 wt.%, between 1 wt. % to 2 wt. %, between 2 wt. % to 3 wt. %, between 3 wt.% to 4 wt. %, between 4 wt. % to 5 wt. %, between 5 wt. % to 6 wt. %,between 6 wt. % to 7 wt. %, between 7 wt. % to 8 wt. %, between 8 wt. %to 9 wt. %, between 9 wt. % to 10 wt. %, between 10 wt. % to 11 wt. %,between 11 wt. % to 12 wt. %, between 12 wt. % to 13 wt. %, between 13wt. % to 14 wt. %, between 14 wt. % to 15 wt. %, between 15 wt. % to 16wt. %, between 16 wt. % to 17 wt. %, between 17 wt. % to 18 wt. %,between 18 wt. % to 19 wt. %, between 19 wt. % to 20 wt. %, between 20wt. % to 21 wt. %, between 21 wt. % to 22 wt. %, between 22 wt. % to 23wt. %, between 23 wt. % to 24 wt. %, between 24 wt. % to 25 wt. %,between 25 wt. % to 26 wt. %, between 26 wt. % to 27 wt. %, between 27wt. % to 28 wt. %, between 28 wt. % to 29 wt. %, between 29 wt. % to 30wt. %, between 30 wt. % to 31 wt. %, between 31 wt. % to 32 wt. %,between 32 wt. % to 33 wt. %, between 33 wt. % to 34 wt. %, between 34wt. % to 35 wt. %, between 35 wt. % to 36 wt. %, between 36 wt. % to 37wt. %, between 37 wt. % to 38 wt. %, between 38 wt. % to 39 wt. %,between 39 wt. % to 40 wt. %, between 40 wt. % to 41 wt. %, between 41wt. % to 42 wt. %, between 42 wt. % to 43 wt. %, between 43 wt. % to 44wt. %, between 44 wt. % to 45 wt. %, between 45 wt. % to 46 wt. %,between 46 wt. % to 47 wt. %, between 47 wt. % to 48 wt. %, between 48wt. % to 49 wt. %, or between 49 wt. % to 50 wt. %.

In an embodiment, a moisturizer composition further includes an amountof vitamin E, or a derivative thereof, of less than 50 wt. %, less than40 wt. %, less than 30 wt. %, less than 20 wt. %, less than 19.75 wt. %,less than 19.50 wt. %, less than 19.25 wt. %, less than 19 wt. %, lessthan 18.75 wt. %, less than 18.50 wt. %, less than 18.25 wt. %, lessthan 18 wt. %, less than 17.75 wt. %, less than 17.50 wt. %, less than17.25 wt. %, less than 17 wt. %, less than 16.75 wt. %, less than 16.50wt. %, less than 16.25 wt. % less than 16 wt. %, less than 15.75 wt. %,less than 15.50 wt. %, less than 15.25 wt. %, less than 15 wt. %, lessthan 14.75 wt. %, less than 14.50 wt. %, less than 14.25 wt. %, lessthan 14 wt. %, less than 13.75 wt. %, less than 13.50 wt. %, less than13.25 wt. %, less than 13 wt. %, less than 12.75 wt. %, less than 12.50wt. %, less than 12.25 wt. %, less than 12 wt. %, less than 11.75 wt. %,less than 11.50 wt. %, less than 11.25 wt. %, less than 11 wt. %, lessthan 10.75 wt. %, less than 10.50 wt. %, less than 10.25 wt. %, lessthan 10 wt. %, less than 9.75 wt. %, less than 9.50 wt. %, less than9.25 wt. %, less than 9 wt. %, less than 8.75 wt. %, less than 8.50 wt.%, less than 8.25 wt. %, less than 8 wt. %, less than 7.75 wt. %, lessthan 7.50 wt. %, less than 7.25 wt. %, less than 7 wt. %, less than 6.75wt. %, less than 6.50 wt. %, less than 6.25 wt. %, less than 6 wt. %,less than 5.75 wt. %, less than 5.50 wt. %, less than 5.25 wt. %, lessthan 5 wt. %, less than 4.75 wt. %, less than 4.50 wt. %, less than 4.25wt. %, less than 4 wt. %, less than 3.75 wt. %, less than 3.50 wt. %,less than 3.25 wt. %, less than 3 wt. %, less than 2.75 wt. %, less than2.50 wt. %, less than 2.25 wt. %, less than 2 wt. %, less than 1.75 wt.%, less than 1.50 wt. %, less than 1.25 wt. %, less than 1 wt. %, lessthan 0.5 wt. %, less than 0.4 wt. %, less than 0.3 wt. %, less than 0.2wt. %, less than 0.1 wt. %, less than 0.09 wt. %, less than 0.08 wt. %,less than 0.07 wt. %, less than 0.06 wt. %, less than 0.05 wt. %, lessthan 0.04 wt. %, less than 0.03 wt. %, less than 0.02 wt. %, less than0.01 wt. %, less than 0.009 wt. %, less than 0.008 wt. %, less than0.007 wt. %, less than 0.006 wt. %, less than 0.005 wt. %, less than0.004 wt. %, less than 0.003 wt. %, less than 0.002 wt. %, or less than0.001 wt. %.

In an embodiment, the moisturizer composition further includes an amountof vitamin E, or a derivative thereof, of greater than 45 wt. %, greaterthan 40 wt. %, greater than 30 wt. %, greater than 20 wt. %, greaterthan 19.75 wt. %, greater than 19.50 wt. %, greater than 19.25 wt. %,greater than 19 wt. %, greater than 18.75 wt. %, greater than 18.50 wt.%, greater than 18.25 wt. %, greater than 18 wt. %, greater than 17.75wt. %, greater than 17.50 wt. %, greater than 17.25 wt. %, greater than17 wt. %, greater than 16.75 wt. %, greater than 16.50 wt. %, greaterthan 16.25 wt. % greater than 16 wt. %, greater than 15.75 wt. %,greater than 15.50 wt. %, greater than 15.25 wt. %, greater than 15 wt.%, greater than 14.75 wt. %, greater than 14.50 wt. %, greater than14.25 wt. %, greater than 14 wt. %, greater than 13.75 wt. %, greaterthan 13.50 wt. %, greater than 13.25 wt. %, greater than 13 wt. %,greater than 12.75 wt. %, greater than 12.50 wt. %, greater than 12.25wt. %, greater than 12 wt. %, greater than 11.75 wt. %, greater than11.50 wt. %, greater than 11.25 wt. %, greater than 11 wt. %, greaterthan 10.75 wt. %, greater than 10.50 wt. %, greater than 10.25 wt. %,greater than 10 wt. %, greater than 9.75 wt. %, greater than 9.50 wt. %,greater than 9.25 wt. %, greater than 9 wt. %, greater than 8.75 wt. %,greater than 8.50 wt. %, greater than 8.25 wt. %, greater than 8 wt. %,greater than 7.75 wt. %, greater than 7.50 wt. %, greater than 7.25 wt.%, greater than 7 wt. %, greater than 6.75 wt. %, greater than 6.50 wt.%, greater than 6.25 wt. %, greater than 6 wt. %, greater than 5.75 wt.%, greater than 5.50 wt. %, greater than 5.25 wt. %, greater than 5 wt.%, greater than 4.75 wt. %, greater than 4.50 wt. %, greater than 4.25wt. %, greater than 4 wt. %, greater than 3.75 wt. %, greater than 3.50wt. %, greater than 3.25 wt. %, greater than 3 wt. %, greater than 2.75wt. %, greater than 2.50 wt. %, greater than 2.25 wt. %, greater than 2wt. %, greater than 1.75 wt. %, greater than 1.50 wt. %, greater than1.25 wt. %, greater than 1 wt. %, greater than 0.5 wt. %, greater than0.4 wt. %, greater than 0.3 wt. %, greater than 0.2 wt. %, greater than0.1 wt. %, greater than 0.09 wt. %, greater than 0.08 wt. %, greaterthan 0.07 wt. %, greater than 0.06 wt. %, greater than 0.05 wt. %,greater than 0.04 wt. %, greater than 0.03 wt. %, greater than 0.02 wt.%, greater than 0.01 wt. %, greater than 0.009 wt. %, greater than 0.008wt. %, greater than 0.007 wt. %, greater than 0.006 wt. %, greater than0.005 wt. %, greater than 0.004 wt. %, greater than 0.003 wt. %, greaterthan 0.002 wt. %, or greater than 0.001 wt. %.

In an embodiment, the invention includes compositions that are stablewater-in-oil (w/o) emulsions comprising water, oil, and silk proteinfragment solutions. In an embodiment, the invention includescompositions that are stable oil-in-water (o/w) emulsions comprisingwater, oil, and silk protein fragment solutions. In an embodiment, theinvention includes compositions that are stable emulsions. The term“stable emulsion” refers to an emulsion that does not undergo phaseseparation upon storage. In an embodiment, a stable solution does notundergo phase separation for at least 1 day, at least 2 days, at least 4days, at least 1 week, at least 2 weeks, at least 1 month, at least 2months, at least 6 months, and at least 1 year.

In an embodiment, the invention includes compositions that are in theform of a liquid, semisolid, or solid. In some embodiments, theinvention includes compositions that are in the form of lotions, creams,oils, gels, emulsions, sticks, sprays, ointments, pastes, mousses,foams, or suspensions. In an embodiment, the invention includescompositions that are in the form of a sunscreen, a cleanser, a bar ofsoap, a lip balm, a foot balm, a deodorant stick, an antiperspirantstick, a liquid or spray deodorant, a liquid or spray antiperspirant, ahair conditioner, and a shampoo. Nevertheless, it is understood to bewithin the scope of the invention that any of the foregoing compositionsmay be prepared with elements of other compositions of the inventionsuch as, without limitation, silk, hyaluronic acid, and one or moreemollients as described herein.

In an embodiment, the invention includes compositions that may beshampoos. For example, the shampoos of the invention may include adetergent, soap, and/or a surfactant, including, without limitation,fatty acids (e.g., one or more of lauric acid, myristic acid, stearicacid, and oleic acid) and/or a lauryl/laureth sulfate (e.g., sodiumlauryl/laureth sulfate, ammonium lauryl sulfate).

In an embodiment, the invention includes compositions that may beconditioners. For example, the conditioners of the invention may includeone or more conditioning agents. Conditioning agents may includeglycerol, propylene glycol, erithritol, sodium PCA, hyaluronic acid,sorbitol, fructose, fatty acids (e.g., stearic acid and oleic acid),fatty alcohols, sorbitol, fructose, a polyquaternium polymer, a cationicsurfactant, proteins, amino acids, oils, mineral oil, silicons, fattyacid esters, glycerin, cetrimonium chloride, fatty alcohols, anddimethicone.

In an embodiment, the invention includes compositions that may bedeodorants and/or antiperspirants. The deodorants and/or antiperspirantsof the invention may include one or more of an aluminum based compound,mineral salts (e.g., aluminum mineral salts), talcum powder, sodiumbicarbonate, sodium stearate, witch hazel, baking soda, hops, aloe vera,and one or more essential oils that provide antibacterial and/orantifungal properties (e.g., lemongrass oil, eucalyptus oil, tea treeoil, and rosemary oil). The aluminum based compound may include one ormore of aluminum chloride, aluminum chlorohydrate, aluminum-zirconiumcompounds, aluminum zirconium tetrachlorohydrex gly, aluminum zirconiumtrichlorohydrex gly, aluminum sesquichlorohydrate, and aluminumsesquichlorohydrex compounds. The mineral salts may include one or moreof potassium alum and ammonium alum.

Sunscreen

The compositions of the invention (e.g., moisturizer compositions) mayinclude a sunscreen or sunblock. For example, the sunscreen or sunblockmay include one or more of a physical UV blocker and a chemical UVblocker. The physical UV blockers may include one or more of titaniumdioxide, zinc oxide, micronized titanium dioxide, micronized zinc oxide,and oil soluble zinc oxide. The chemical UV blockers may include one ormore of octylcrylene, avobenzone, octinoxate, octisalate, oxybenzone,homosalate, helioplex, 4-MBC, mexoryl SX and XL, tinosorb S and M,uvinul T 150, and uvinul A plus.

In an embodiment, a moisturizer composition further includes an amountof a sunscreen of about 50 wt. %, about 45 wt. %, about 40 wt. %, about35 wt. %, about 30 wt. %, about 25 wt. %, about 20 wt. %, about 19.75wt. %, about 19.50 wt. %, about 19.25 wt. %, about 19 wt. %, about 18.75wt. %, about 18.50 wt. %, about 18.25 wt. %, about 18 wt. %, about 17.75wt. %, about 17.50 wt. %, about 17.25 wt. %, about 17 wt. %, about 16.75wt. %, about 16.50 wt. %, about 16.25 wt. % about 16 wt. %, about 15.75wt. %, about 15.50 wt. %, about 15.25 wt. %, about 15 wt. %, about 14.75wt. %, about 14.50 wt. %, about 14.25 wt. %, about 14 wt. %, about 13.75wt. %, about 13.50 wt. %, about 13.25 wt. %, about 13 wt. %, about 12.75wt. %, about 12.50 wt. %, about 12.25 wt. %, about 12 wt. %, about 11.75wt. %, about 11.50 wt. %, about 11.25 wt. %, about 11 wt. %, about 10.75wt. %, about 10.50 wt. %, about 10.25 wt. %, about 10 wt. %, about 9.75wt. %, about 9.50 wt. %, about 9.25 wt. %, about 9 wt. %, about 8.75 wt.%, about 8.50 wt. %, about 8.25 wt. %, about 8 wt. %, about 7.75 wt. %,about 7.50 wt. %, about 7.25 wt. %, about 7 wt. %, about 6.75 wt. %,about 6.50 wt. %, about 6.25 wt. %, about 6 wt. %, about 5.75 wt. %,about 5.50 wt. %, about 5.25 wt. %, about 5 wt. %, about 4.75 wt. %,about 4.50 wt. %, about 4.25 wt. %, about 4 wt. %, about 3.75 wt. %,about 3.50 wt. %, about 3.25 wt. %, about 3 wt. %, about 2.75 wt. %,about 2.50 wt. %, about 2.25 wt. %, about 2 wt. %, about 1.75 wt. %,about 1.50 wt. %, about 1.25 wt. %, about 1 wt. %, about 0.5 wt. %,about 0.4 wt. %, about 0.3 wt. %, about 0.2 wt. %, about 0.1 wt. %,about 0.09 wt. %, about 0.08 wt. %, about 0.07 wt. %, about 0.06 wt. %,about 0.05 wt. %, about 0.04 wt. %, about 0.03 wt. %, about 0.02 wt. %,about 0.01 wt. %, about 0.009 wt. %, about 0.008 wt. %, about 0.007 wt.%, about 0.006 wt. %, about 0.005 wt. %, about 0.004 wt. %, about 0.003wt. %, about 0.002 wt. %, or about 0.001 wt. %.

In an embodiment, a moisturizer composition further includes an amountof a sunscreen of between about 1 wt. % to about 50 wt. %, between about2 wt. % to about 40 wt. %, between about 3 wt. % to about 30 wt. %,between about 4 wt. % to about 20 wt. %, between about 5 wt. % to about15 wt. %, between about 6 wt. % to about 10 wt. %, between about 7 wt. %to about 9 wt. %, between about 10 wt. % to about 50 wt. %, betweenabout 15 wt. % to about 45 wt. %, between about 20 wt. % to about 40 wt.%, between about 25 wt. % to about 35 wt. %, or between about 25 wt. %to about 30 wt. %.

In an embodiment, a moisturizer composition further includes an amountof a sunscreen of between about 0.001 wt. % to about 5 wt. %, betweenabout 5 wt. % to about 10 wt. %, between about 10 wt. % to about 15 wt.%, between about 15 wt. % to about 20 wt. %, between about 20 wt. % toabout 25 wt. %, between about 25 wt. % to about 30 wt. %, between about30 wt. % to about 35 wt. %, between about 35 wt. % to about 40 wt. %,between about 40 wt. % to about 45 wt. %, or between about 45 wt. % toabout 50 wt. %.

In an embodiment, a moisturizer composition further includes an amountof a sunscreen of between about 0.001 wt. % to about 1 wt. %, betweenabout 1 wt. % to about 2 wt. %, between about 2 wt. % to about 3 wt. %,between about 3 wt. % to about 4 wt. %, between about 4 wt. % to about 5wt. %, between about 5 wt. % to about 6 wt. %, between about 6 wt. % toabout 7 wt. %, between about 7 wt. % to about 8 wt. %, between about 8wt. % to about 9 wt. %, between about 9 wt. % to about 10 wt. %, betweenabout 10 wt. % to about 11 wt. %, between about 11 wt. % to about 12 wt.%, between about 12 wt. % to about 13 wt. %, between about 13 wt. % toabout 14 wt. %, between about 14 wt. % to about 15 wt. %, between about15 wt. % to about 16 wt. %, between about 16 wt. % to about 17 wt. %,between about 17 wt. % to about 18 wt. %, between about 18 wt. % toabout 19 wt. %, between about 19 wt. % to about 20 wt. %, between about20 wt. % to about 21 wt. %, between about 21 wt. % to about 22 wt. %,between about 22 wt. % to about 23 wt. %, between about 23 wt. % toabout 24 wt. %, between about 24 wt. % to about 25 wt. %, between about25 wt. % to about 26 wt. %, between about 26 wt. % to about 27 wt. %,between about 27 wt. % to about 28 wt. %, between about 28 wt. % toabout 29 wt. %, between about 29 wt. % to about 30 wt. %, between about30 wt. % to about 31 wt. %, between about 31 wt. % to about 32 wt. %,between about 32 wt. % to about 33 wt. %, between about 33 wt. % toabout 34 wt. %, between about 34 wt. % to about 35 wt. %, between about35 wt. % to about 36 wt. %, between about 36 wt. % to about 37 wt. %,between about 37 wt. % to about 38 wt. %, between about 38 wt. % toabout 39 wt. %, between about 39 wt. % to about 40 wt. %, between about40 wt. % to about 41 wt. %, between about 41 wt. % to about 42 wt. %,between about 42 wt. % to about 43 wt. %, between about 43 wt. % toabout 44 wt. %, between about 44 wt. % to about 45 wt. %, between about45 wt. to about 46 wt. %, between about 46 wt. % to about 47 wt. %,between about 47 wt. % to about 48 wt. %, between about 48 wt. % toabout 49 wt. %, or between about 49 wt. % to about 50 wt. %.

In an embodiment, a moisturizer composition further includes an amountof a sunscreen of 50 wt. %, 45 wt. %, 40 wt. %, 35 wt. %, 30 wt. %, 25wt. %, 20 wt. %, 19.75 wt. %, 19.50 wt. %, 19.25 wt. %, 19 wt. %, 18.75wt. %, 18.50 wt. %, 18.25 wt. %, 18 wt. %, 17.75 wt. %, 17.50 wt. %,17.25 wt. %, 17 wt. %, 16.75 wt. %, 16.50 wt. %, 16.25 wt. % 16 wt. %,15.75 wt. %, 15.50 wt. %, 15.25 wt. %, 15 wt. %, 14.75 wt. %, 14.50 wt.%, 14.25 wt. %, 14 wt. %, 13.75 wt. %, 13.50 wt. %, 13.25 wt. %, 13 wt.%, 12.75 wt. %, 12.50 wt. %, 12.25 wt. %, 12 wt. %, 11.75 wt. %, 11.50wt. %, 11.25 wt. %, 11 wt. %, 10.75 wt. %, 10.50 wt. %, 10.25 wt. %, 10wt. %, 9.75 wt. %, 9.50 wt. %, 9.25 wt. %, 9 wt. %, 8.75 wt. %, 8.50 wt.%, 8.25 wt. %, 8 wt. %, 7.75 wt. %, 7.50 wt. %, 7.25 wt. %, 7 wt. %,6.75 wt. %, 6.50 wt. %, 6.25 wt. %, 6 wt. %, 5.75 wt. %, 5.50 wt. %,5.25 wt. %, 5 wt. %, 4.75 wt. %, 4.50 wt. %, 4.25 wt. %, 4 wt. %, 3.75wt. %, 3.50 wt. %, 3.25 wt. %, 3 wt. %, 2.75 wt. %, 2.50 wt. %, 2.25 wt.%, 2 wt. %, 1.75 wt. %, 1.50 wt. %, 1.25 wt. %, 1 wt. %, 0.5 wt. %, 0.4wt. %, 0.3 wt. %, 0.2 wt. %, 0.1 wt. %, 0.09 wt. %, 0.08 wt. %, 0.07 wt.%, 0.06 wt. %, 0.05 wt. %, 0.04 wt. %, 0.03 wt. %, 0.02 wt. %, 0.01 wt.%, 0.009 wt. %, 0.008 wt. %, 0.007 wt. %, 0.006 wt. %, 0.005 wt. %,0.004 wt. %, 0.003 wt. %, 0.002 wt. %, or 0.001 wt. %.

In an embodiment, a moisturizer composition further includes an amountof a sunscreen of between 1 wt. % to 50 wt. %, between 2 wt. % to 40 wt.%, between 3 wt. % to 30 wt. %, between 4 wt. % to 20 wt. %, between 5wt. % to 15 wt. %, between 6 wt. % to 10 wt. %, between 7 wt. % to 9 wt.%, between 10 wt. % to 50 wt. %, between 15 wt. % to 45 wt. %, between20 wt. % to 40 wt. %, between 25 wt. % to 35 wt. %, or between 30 wt. %to 35 wt. %.

In an embodiment, a moisturizer composition further includes an amountof a sunscreen of between 0.001 wt. % to 5 wt. %, between 5 wt. % to 10wt. %, between 10 wt. % to 15 wt. %, between 15 wt. % to 20 wt. %,between 20 wt. % to 25 wt. %, between 25 wt. % to 30 wt. %, between 30wt. % to 35 wt. %, between 35 wt. % to 40 wt. %, between 40 wt. % to 45wt. %, or between 45 wt. % to 50 wt. %.

In an embodiment, a moisturizer composition further includes an amountof a sunscreen of between 0.001 wt. % to 1 wt. %, between 1 wt. % to 2wt. %, between 2 wt. % to 3 wt. %, between 3 wt. % to 4 wt. %, between 4wt. % to 5 wt. %, between 5 wt. % to 6 wt. %, between 6 wt. to 7 wt. %,between 7 wt. % to 8 wt. %, between 8 wt. % to 9 wt. %, between 9 wt. %to 10 wt. %, between 10 wt. % to 11 wt. %, between 11 wt. % to 12 wt. %,between 12 wt. % to 13 wt. %, between 13 wt. % to 14 wt. %, between 14wt. % to 15 wt. %, between 15 wt. % to 16 wt. %, between 16 wt. % to 17wt. %, between 17 wt. % to 18 wt. %, between 18 wt. % to 19 wt. %,between 19 wt. % to 20 wt. %, between 20 wt. % to 21 wt. %, between 21wt. % to 22 wt. %, between 22 wt. % to 23 wt. %, between 23 wt. % to 24wt. %, between 24 wt. % to 25 wt. %, between 25 wt. % to 26 wt. %,between 26 wt. % to 27 wt. %, between 27 wt. % to 28 wt. %, between 28wt. % to 29 wt. %, between 29 wt. % to 30 wt. %, between 30 wt. % to 31wt. %, between 31 wt. % to 32 wt. %, between 32 wt. % to 33 wt. %,between 33 wt. % to 34 wt. %, between 34 wt. % to 35 wt. %, between 35wt. % to 36 wt. %, between 36 wt. % to 37 wt. %, between 37 wt. % to 38wt. %, between 38 wt. % to 39 wt. %, between 39 wt. % to 40 wt. %,between 40 wt. % to 41 wt. %, between 41 wt. % to 42 wt. %, between 42wt. % to 43 wt. %, between 43 wt. % to 44 wt. %, between 44 wt. % to 45wt. %, between 45 wt. % to 46 wt. %, between 46 wt. % to 47 wt. %,between 47 wt. % to 48 wt. %, between 48 wt. % to 49 wt. %, or between49 wt. % to 50 wt. %.

In an embodiment, a moisturizer composition further includes an amountof a sunscreen of less than 50 wt. %, less than 40 wt. %, less than 30wt. %, less than 20 wt. %, less than 19.75 wt. %, less than 19.50 wt. %,less than 19.25 wt. %, less than 19 wt. %, less than 18.75 wt. %, lessthan 18.50 wt. %, less than 18.25 wt. %, less than 18 wt. %, less than17.75 wt. %, less than 17.50 wt. %, less than 17.25 wt. %, less than 17wt. %, less than 16.75 wt. %, less than 16.50 wt. %, less than 16.25 wt.% less than 16 wt. %, less than 15.75 wt. %, less than 15.50 wt. %, lessthan 15.25 wt. %, less than 15 wt. %, less than 14.75 wt. %, less than14.50 wt. %, less than 14.25 wt. %, less than 14 wt. %, less than 13.75wt. %, less than 13.50 wt. %, less than 13.25 wt. %, less than 13 wt. %,less than 12.75 wt. %, less than 12.50 wt. %, less than 12.25 wt. %,less than 12 wt. %, less than 11.75 wt. %, less than 11.50 wt. %, lessthan 11.25 wt. %, less than 11 wt. %, less than 10.75 wt. %, less than10.50 wt. %, less than 10.25 wt. %, less than 10 wt. %, less than 9.75wt. %, less than 9.50 wt. %, less than 9.25 wt. %, less than 9 wt. %,less than 8.75 wt. %, less than 8.50 wt. %, less than 8.25 wt. %, lessthan 8 wt. %, less than 7.75 wt. %, less than 7.50 wt. %, less than 7.25wt. %, less than 7 wt. %, less than 6.75 wt. %, less than 6.50 wt. %,less than 6.25 wt. %, less than 6 wt. %, less than 5.75 wt. %, less than5.50 wt. %, less than 5.25 wt. %, less than 5 wt. %, less than 4.75 wt.%, less than 4.50 wt. %, less than 4.25 wt. %, less than 4 wt. %, lessthan 3.75 wt. %, less than 3.50 wt. %, less than 3.25 wt. %, less than 3wt. %, less than 2.75 wt. %, less than 2.50 wt. %, less than 2.25 wt. %,less than 2 wt. %, less than 1.75 wt. %, less than 1.50 wt. %, less than1.25 wt. %, less than 1 wt. %, less than 0.5 wt. %, less than 0.4 wt. %,less than 0.3 wt. %, less than 0.2 wt. %, less than 0.1 wt. %, less than0.09 wt. %, less than 0.08 wt. %, less than 0.07 wt. %, less than 0.06wt. %, less than 0.05 wt. %, less than 0.04 wt. %, less than 0.03 wt. %,less than 0.02 wt. %, less than 0.01 wt. %, less than 0.009 wt. %, lessthan 0.008 wt. %, less than 0.007 wt. %, less than 0.006 wt. %, lessthan 0.005 wt. %, less than 0.004 wt. %, less than 0.003 wt. %, lessthan 0.002 wt. %, or less than 0.001 wt. %.

In an embodiment, the moisturizer composition further includes an amountof a sunscreen of greater than 45 wt. %, greater than 40 wt. %, greaterthan 30 wt. %, greater than 20 wt. %, greater than 19.75 wt. %, greaterthan 19.50 wt. %, greater than 19.25 wt. %, greater than 19 wt. %,greater than 18.75 wt. %, greater than 18.50 wt. %, greater than 18.25wt. %, greater than 18 wt. %, greater than 17.75 wt. %, greater than17.50 wt. %, greater than 17.25 wt. %, greater than 17 wt. %, greaterthan 16.75 wt. %, greater than 16.50 wt. %, greater than 16.25 wt. %greater than 16 wt. %, greater than 15.75 wt. %, greater than 15.50 wt.%, greater than 15.25 wt. %, greater than 15 wt. %, greater than 14.75wt. %, greater than 14.50 wt. %, greater than 14.25 wt. %, greater than14 wt. %, greater than 13.75 wt. %, greater than 13.50 wt. %, greaterthan 13.25 wt. %, greater than 13 wt. %, greater than 12.75 wt. %,greater than 12.50 wt. %, greater than 12.25 wt. %, greater than 12 wt.%, greater than 11.75 wt. %, greater than 11.50 wt. %, greater than11.25 wt. %, greater than 11 wt. %, greater than 10.75 wt. %, greaterthan 10.50 wt. %, greater than 10.25 wt. %, greater than 10 wt. %,greater than 9.75 wt. %, greater than 9.50 wt. %, greater than 9.25 wt.%, greater than 9 wt. %, greater than 8.75 wt. %, greater than 8.50 wt.%, greater than 8.25 wt. %, greater than 8 wt. %, greater than 7.75 wt.%, greater than 7.50 wt. %, greater than 7.25 wt. %, greater than 7 wt.%, greater than 6.75 wt. %, greater than 6.50 wt. %, greater than 6.25wt. %, greater than 6 wt. %, greater than 5.75 wt. %, greater than 5.50wt. %, greater than 5.25 wt. %, greater than 5 wt. %, greater than 4.75wt. %, greater than 4.50 wt. %, greater than 4.25 wt. %, greater than 4wt. %, greater than 3.75 wt. %, greater than 3.50 wt. %, greater than3.25 wt. %, greater than 3 wt. %, greater than 2.75 wt. %, greater than2.50 wt. %, greater than 2.25 wt. %, greater than 2 wt. %, greater than1.75 wt. %, greater than 1.50 wt. %, greater than 1.25 wt. %, greaterthan 1 wt. %, greater than 0.5 wt. %, greater than 0.4 wt. %, greaterthan 0.3 wt. %, greater than 0.2 wt. %, greater than 0.1 wt. %, greaterthan 0.09 wt. %, greater than 0.08 wt. %, greater than 0.07 wt. %,greater than 0.06 wt. %, greater than 0.05 wt. %, greater than 0.04 wt.%, greater than 0.03 wt. %, greater than 0.02 wt. %, greater than 0.01wt. %, greater than 0.009 wt. %, greater than 0.008 wt. %, greater than0.007 wt. %, greater than 0.006 wt. %, greater than 0.005 wt. %, greaterthan 0.004 wt. %, greater than 0.003 wt. %, greater than 0.002 wt. %, orgreater than 0.001 wt. %.

In an embodiment, a sunscreen has a sun protection factor of 5, 10, 15,20, 25, 30, 35, 40, 45, or 50. In an embodiment, a sunscreen has a sunprotection factor of 5 to 10, 10 to 15, 15 to 20, 20 to 25, 25 to 30, 30to 35, 35 to 40, 40 to 45, or 45 to 50. In an embodiment, a sunscreenhas a sun protection factor of greater than 5, greater than 10, greaterthan 15, greater than 20, greater than 25, greater than 30, greater than35, greater than 40, greater than 45, or greater than 50. In anembodiment, a sunscreen has a sun protection factor of less than 5, lessthan 10, less than 15, less than 20, less than 25, less than 30, lessthan 35, less than 40, less than 45, or less than 50.

In an embodiment, a moisturizer composition further includes an amountof a sunblock of about 50 wt. %, about 45 wt. %, about 40 wt. %, about35 wt. %, about 30 wt. %, about 25 wt. %, about 20 wt. %, about 19.75wt. %, about 19.50 wt. %, about 19.25 wt. %, about 19 wt. %, about 18.75wt. %, about 18.50 wt. %, about 18.25 wt. %, about 18 wt. %, about 17.75wt. %, about 17.50 wt. %, about 17.25 wt. %, about 17 wt. %, about 16.75wt. %, about 16.50 wt. %, about 16.25 wt. % about 16 wt. %, about 15.75wt. %, about 15.50 wt. %, about 15.25 wt. %, about 15 wt. %, about 14.75wt. %, about 14.50 wt. %, about 14.25 wt. %, about 14 wt. %, about 13.75wt. %, about 13.50 wt. %, about 13.25 wt. %, about 13 wt. %, about 12.75wt. %, about 12.50 wt. %, about 12.25 wt. %, about 12 wt. %, about 11.75wt. %, about 11.50 wt. %, about 11.25 wt. %, about 11 wt. %, about 10.75wt. %, about 10.50 wt. %, about 10.25 wt. %, about 10 wt. %, about 9.75wt. %, about 9.50 wt. %, about 9.25 wt. %, about 9 wt. %, about 8.75 wt.%, about 8.50 wt. %, about 8.25 wt. %, about 8 wt. %, about 7.75 wt. %,about 7.50 wt. %, about 7.25 wt. %, about 7 wt. %, about 6.75 wt. %,about 6.50 wt. %, about 6.25 wt. %, about 6 wt. %, about 5.75 wt. %,about 5.50 wt. %, about 5.25 wt. %, about 5 wt. %, about 4.75 wt. %,about 4.50 wt. %, about 4.25 wt. %, about 4 wt. %, about 3.75 wt. %,about 3.50 wt. %, about 3.25 wt. %, about 3 wt. %, about 2.75 wt. %,about 2.50 wt. %, about 2.25 wt. %, about 2 wt. %, about 1.75 wt. %,about 1.50 wt. %, about 1.25 wt. %, about 1 wt. %, about 0.5 wt. %,about 0.4 wt. %, about 0.3 wt. %, about 0.2 wt. %, about 0.1 wt. %,about 0.09 wt. %, about 0.08 wt. %, about 0.07 wt. %, about 0.06 wt. %,about 0.05 wt. %, about 0.04 wt. %, about 0.03 wt. %, about 0.02 wt. %,about 0.01 wt. %, about 0.009 wt. %, about 0.008 wt. %, about 0.007 wt.%, about 0.006 wt. %, about 0.005 wt. %, about 0.004 wt. %, about 0.003wt. %, about 0.002 wt. %, or about 0.001 wt. %.

In an embodiment, a moisturizer composition further includes an amountof a sunblock of between about 1 wt. % to about 50 wt. %, between about2 wt. % to about 40 wt. %, between about 3 wt. % to about 30 wt. %,between about 4 wt. % to about 20 wt. %, between about 5 wt. % to about15 wt. %, between about 6 wt. % to about 10 wt. %, between about 7 wt. %to about 9 wt. %, between about 10 wt. % to about 50 wt. %, betweenabout 15 wt. % to about 45 wt. %, between about 20 wt. % to about 40 wt.%, between about 25 wt. % to about 35 wt. %, or between about 25 wt. %to about 30 wt. %.

In an embodiment, a moisturizer composition further includes an amountof a sunblock of between about 0.001 wt. % to about 5 wt. %, betweenabout 5 wt. % to about 10 wt. %, between about 10 wt. % to about 15 wt.%, between about 15 wt. % to about 20 wt. %, between about 20 wt. % toabout 25 wt. %, between about 25 wt. % to about 30 wt. %, between about30 wt. % to about 35 wt. %, between about 35 wt. % to about 40 wt. %,between about 40 wt. % to about 45 wt. %, or between about 45 wt. % toabout 50 wt. %.

In an embodiment, a moisturizer composition further includes an amountof a sunblock of between about 0.001 wt. % to about 1 wt. %, betweenabout 1 wt. % to about 2 wt. %, between about 2 wt. % to about 3 wt. %,between about 3 wt. % to about 4 wt. %, between about 4 wt. % to about 5wt. %, between about 5 wt. % to about 6 wt. %, between about 6 wt. % toabout 7 wt. %, between about 7 wt. % to about 8 wt. %, between about 8wt. % to about 9 wt. %, between about 9 wt. % to about 10 wt. %, betweenabout 10 wt. % to about 11 wt. %, between about 11 wt. % to about 12 wt.%, between about 12 wt. % to about 13 wt. %, between about 13 wt. % toabout 14 wt. %, between about 14 wt. % to about 15 wt. %, between about15 wt. % to about 16 wt. %, between about 16 wt. % to about 17 wt. %,between about 17 wt. % to about 18 wt. %, between about 18 wt. % toabout 19 wt. %, between about 19 wt. % to about 20 wt. %, between about20 wt. % to about 21 wt. %, between about 21 wt. % to about 22 wt. %,between about 22 wt. % to about 23 wt. %, between about 23 wt. % toabout 24 wt. %, between about 24 wt. % to about 25 wt. %, between about25 wt. % to about 26 wt. %, between about 26 wt. % to about 27 wt. %,between about 27 wt. % to about 28 wt. %, between about 28 wt. % toabout 29 wt. %, between about 29 wt. % to about 30 wt. %, between about30 wt. % to about 31 wt. %, between about 31 wt. % to about 32 wt. %,between about 32 wt. % to about 33 wt. %, between about 33 wt. % toabout 34 wt. %, between about 34 wt. % to about 35 wt. %, between about35 wt. % to about 36 wt. %, between about 36 wt. % to about 37 wt. %,between about 37 wt. % to about 38 wt. %, between about 38 wt. % toabout 39 wt. %, between about 39 wt. % to about 40 wt. %, between about40 wt. % to about 41 wt. %, between about 41 wt. % to about 42 wt. %,between about 42 wt. % to about 43 wt. %, between about 43 wt. % toabout 44 wt. %, between about 44 wt. % to about 45 wt. %, between about45 wt. % to about 46 wt. %, between about 46 wt. % to about 47 wt. %,between about 47 wt. % to about 48 wt. %, between about 48 wt. % toabout 49 wt. %, or between about 49 wt. % to about 50 wt. %.

In an embodiment, a moisturizer composition further includes an amountof a sunblock of 50 wt. %, 45 wt. %, 40 wt. %, 35 wt. %, 30 wt. %, 25wt. %, 20 wt. %, 19.75 wt. %, 19.50 wt. %, 19.25 wt. %, 19 wt. %, 18.75wt. %, 18.50 wt. %, 18.25 wt. %, 18 wt. %, 17.75 wt. %, 17.50 wt. %,17.25 wt. %, 17 wt. %, 16.75 wt. %, 16.50 wt. %, 16.25 wt. % 16 wt. %,15.75 wt. %, 15.50 wt. %, 15.25 wt. %, 15 wt. %, 14.75 wt. %, 14.50 wt.%, 14.25 wt. %, 14 wt. %, 13.75 wt. %, 13.50 wt. %, 13.25 wt. %, 13 wt.%, 12.75 wt. %, 12.50 wt. %, 12.25 wt. %, 12 wt. %, 11.75 wt. %, 11.50wt. %, 11.25 wt. %, 11 wt. %, 10.75 wt. %, 10.50 wt. %, 10.25 wt. %, 10wt. %, 9.75 wt. %, 9.50 wt. %, 9.25 wt. %, 9 wt. %, 8.75 wt. %, 8.50 wt.%, 8.25 wt. %, 8 wt. %, 7.75 wt. %, 7.50 wt. %, 7.25 wt. %, 7 wt. %,6.75 wt. %, 6.50 wt. %, 6.25 wt. %, 6 wt. %, 5.75 wt. %, 5.50 wt. %,5.25 wt. %, 5 wt. %, 4.75 wt. %, 4.50 wt. %, 4.25 wt. %, 4 wt. %, 3.75wt. %, 3.50 wt. %, 3.25 wt. %, 3 wt. %, 2.75 wt. %, 2.50 wt. %, 2.25 wt.%, 2 wt. %, 1.75 wt. %, 1.50 wt. %, 1.25 wt. %, 1 wt. %, 0.5 wt. %, 0.4wt. %, 0.3 wt. %, 0.2 wt. %, 0.1 wt. %, 0.09 wt. %, 0.08 wt. %, 0.07 wt.%, 0.06 wt. %, 0.05 wt. %, 0.04 wt. %, 0.03 wt. %, 0.02 wt. %, 0.01 wt.%, 0.009 wt. %, 0.008 wt. %, 0.007 wt. %, 0.006 wt. %, 0.005 wt. %,0.004 wt. %, 0.003 wt. %, 0.002 wt. %, or 0.001 wt. %.

In an embodiment, a moisturizer composition further includes an amountof a sunblock of between 1 wt. % to 50 wt. %, between 2 wt. % to 40 wt.%, between 3 wt. % to 30 wt. %, between 4 wt. % to 20 wt. %, between 5wt. % to 15 wt. %, between 6 wt. % to 10 wt. %, between 7 wt. % to 9 wt.%, between 10 wt. % to 50 wt. %, between 15 wt. % to 45 wt. %, between20 wt. % to 40 wt. %, between 25 wt. % to 35 wt. %, or between 30 wt. %to 35 wt. %.

In an embodiment, a moisturizer composition further includes an amountof a sunblock of between 0.001 wt. % to 5 wt. %, between 5 wt. % to 10wt. %, between 10 wt. % to 15 wt. %, between 15 wt. % to 20 wt. %,between 20 wt. % to 25 wt. %, between 25 wt. % to 30 wt. %, between 30wt. % to 35 wt. %, between 35 wt. % to 40 wt. %, between 40 wt. % to 45wt. %, or between 45 wt. % to 50 wt. %.

In an embodiment, a moisturizer composition further includes an amountof a sunblock of between 0.001 wt. % to 1 wt. %, between 1 wt. % to 2wt. %, between 2 wt. % to 3 wt. %, between 3 wt. % to 4 wt. %, between 4wt. % to 5 wt. %, between 5 wt. % to 6 wt. %, between 6 wt. % to 7 wt.%, between 7 wt. % to 8 wt. %, between 8 wt. % to 9 wt. %, between 9 wt.% to 10 wt. %, between 10 wt. % to 11 wt. %, between 11 wt. % to 12 wt.%, between 12 wt. % to 13 wt. %, between 13 wt. % to 14 wt. %, between14 wt. % to 15 wt. %, between 15 wt. % to 16 wt. %, between 16 wt. % to17 wt. %, between 17 wt. % to 18 wt. %, between 18 wt. % to 19 wt. %,between 19 wt. % to 20 wt. %, between 20 wt. % to 21 wt. %, between 21wt. % to 22 wt. %, between 22 wt. % to 23 wt. %, between 23 wt. % to 24wt. %, between 24 wt. % to 25 wt. %, between 25 wt. % to 26 wt. %,between 26 wt. % to 27 wt. %, between 27 wt. % to 28 wt. %, between 28wt. % to 29 wt. %, between 29 wt. % to 30 wt. %, between 30 wt. % to 31wt. %, between 31 wt. % to 32 wt. %, between 32 wt. % to 33 wt. %,between 33 wt. % to 34 wt. %, between 34 wt. % to 35 wt. %, between 35wt. % to 36 wt. %, between 36 wt. % to 37 wt. %, between 37 wt. % to 38wt. %, between 38 wt. % to 39 wt. %, between 39 wt. % to 40 wt. %,between 40 wt. % to 41 wt. %, between 41 wt. % to 42 wt. %, between 42wt. % to 43 wt. %, between 43 wt. % to 44 wt. %, between 44 wt. % to 45wt. %, between 45 wt. % to 46 wt. %, between 46 wt. % to 47 wt. %,between 47 wt. % to 48 wt. %, between 48 wt. % to 49 wt. %, or between49 wt. % to 50 wt. %.

In an embodiment, a moisturizer composition further includes an amountof a sunblock of less than 50 wt. %, less than 40 wt. %, less than 30wt. %, less than 20 wt. %, less than 19.75 wt. %, less than 19.50 wt. %,less than 19.25 wt. %, less than 19 wt. %, less than 18.75 wt. %, lessthan 18.50 wt. %, less than 18.25 wt. %, less than 18 wt. %, less than17.75 wt. %, less than 17.50 wt. %, less than 17.25 wt. %, less than 17wt. %, less than 16.75 wt. %, less than 16.50 wt. %, less than 16.25 wt.% less than 16 wt. %, less than 15.75 wt. %, less than 15.50 wt. %, lessthan 15.25 wt. %, less than 15 wt. %, less than 14.75 wt. %, less than14.50 wt. %, less than 14.25 wt. %, less than 14 wt. %, less than 13.75wt. %, less than 13.50 wt. %, less than 13.25 wt. %, less than 13 wt. %,less than 12.75 wt. %, less than 12.50 wt. %, less than 12.25 wt. %,less than 12 wt. %, less than 11.75 wt. %, less than 11.50 wt. %, lessthan 11.25 wt. %, less than 11 wt. %, less than 10.75 wt. %, less than10.50 wt. %, less than 10.25 wt. %, less than 10 wt. %, less than 9.75wt. %, less than 9.50 wt. %, less than 9.25 wt. %, less than 9 wt. %,less than 8.75 wt. %, less than 8.50 wt. %, less than 8.25 wt. %, lessthan 8 wt. %, less than 7.75 wt. %, less than 7.50 wt. %, less than 7.25wt. %, less than 7 wt. %, less than 6.75 wt. %, less than 6.50 wt. %,less than 6.25 wt. %, less than 6 wt. %, less than 5.75 wt. %, less than5.50 wt. %, less than 5.25 wt. %, less than 5 wt. %, less than 4.75 wt.%, less than 4.50 wt. %, less than 4.25 wt. %, less than 4 wt. %, lessthan 3.75 wt. %, less than 3.50 wt. %, less than 3.25 wt. %, less than 3wt. %, less than 2.75 wt. %, less than 2.50 wt. %, less than 2.25 wt. %,less than 2 wt. %, less than 1.75 wt. %, less than 1.50 wt. %, less than1.25 wt. %, less than 1 wt. %, less than 0.5 wt. %, less than 0.4 wt. %,less than 0.3 wt. %, less than 0.2 wt. %, less than 0.1 wt. %, less than0.09 wt. %, less than 0.08 wt. %, less than 0.07 wt. %, less than 0.06wt. %, less than 0.05 wt. %, less than 0.04 wt. %, less than 0.03 wt. %,less than 0.02 wt. %, less than 0.01 wt. %, less than 0.009 wt. %, lessthan 0.008 wt. %, less than 0.007 wt. %, less than 0.006 wt. %, lessthan 0.005 wt. %, less than 0.004 wt. %, less than 0.003 wt. %, lessthan 0.002 wt. %, or less than 0.001 wt. %.

In an embodiment, the moisturizer composition further includes an amountof a sunblock of greater than 45 wt. %, greater than 40 wt. %, greaterthan 30 wt. %, greater than 20 wt. %, greater than 19.75 wt. %, greaterthan 19.50 wt. %, greater than 19.25 wt. %, greater than 19 wt. %,greater than 18.75 wt. %, greater than 18.50 wt. %, greater than 18.25wt. %, greater than 18 wt. %, greater than 17.75 wt. %, greater than17.50 wt. %, greater than 17.25 wt. %, greater than 17 wt. %, greaterthan 16.75 wt. %, greater than 16.50 wt. %, greater than 16.25 wt. %greater than 16 wt. %, greater than 15.75 wt. %, greater than 15.50 wt.%, greater than 15.25 wt. %, greater than 15 wt. %, greater than 14.75wt. %, greater than 14.50 wt. %, greater than 14.25 wt. %, greater than14 wt. %, greater than 13.75 wt. %, greater than 13.50 wt. %, greaterthan 13.25 wt. %, greater than 13 wt. %, greater than 12.75 wt. %,greater than 12.50 wt. %, greater than 12.25 wt. %, greater than 12 wt.%, greater than 11.75 wt. %, greater than 11.50 wt. %, greater than11.25 wt. %, greater than 11 wt. %, greater than 10.75 wt. %, greaterthan 10.50 wt. %, greater than 10.25 wt. %, greater than 10 wt. %,greater than 9.75 wt. %, greater than 9.50 wt. %, greater than 9.25 wt.%, greater than 9 wt. %, greater than 8.75 wt. %, greater than 8.50 wt.%, greater than 8.25 wt. %, greater than 8 wt. %, greater than 7.75 wt.%, greater than 7.50 wt. %, greater than 7.25 wt. %, greater than 7 wt.%, greater than 6.75 wt. %, greater than 6.50 wt. %, greater than 6.25wt. %, greater than 6 wt. %, greater than 5.75 wt. %, greater than 5.50wt. %, greater than 5.25 wt. %, greater than 5 wt. %, greater than 4.75wt. %, greater than 4.50 wt. %, greater than 4.25 wt. %, greater than 4wt. %, greater than 3.75 wt. %, greater than 3.50 wt. %, greater than3.25 wt. %, greater than 3 wt. %, greater than 2.75 wt. %, greater than2.50 wt. %, greater than 2.25 wt. %, greater than 2 wt. %, greater than1.75 wt. %, greater than 1.50 wt. %, greater than 1.25 wt. %, greaterthan 1 wt. %, greater than 0.5 wt. %, greater than 0.4 wt. %, greaterthan 0.3 wt. %, greater than 0.2 wt. %, greater than 0.1 wt. %, greaterthan 0.09 wt. %, greater than 0.08 wt. %, greater than 0.07 wt. %,greater than 0.06 wt. %, greater than 0.05 wt. %, greater than 0.04 wt.%, greater than 0.03 wt. %, greater than 0.02 wt. %, greater than 0.01wt. %, greater than 0.009 wt. %, greater than 0.008 wt. %, greater than0.007 wt. %, greater than 0.006 wt. %, greater than 0.005 wt. %, greaterthan 0.004 wt. %, greater than 0.003 wt. %, greater than 0.002 wt. %, orgreater than 0.001 wt. %.

In an embodiment, a sunblock has a sun protection factor of 5, 10, 15,20, 25, 30, 35, 40, 45, or 50. In an embodiment, a sunblock has a sunprotection factor of 5 to 10, 10 to 15, 15 to 20, 20 to 25, 25 to 30, 30to 35, 35 to 40, 40 to 45, or 45 to 50. In an embodiment, a sunblock hasa sun protection factor of greater than 5, greater than 10, greater than15, greater than 20, greater than 25, greater than 30, greater than 35,greater than 40, greater than 45, or greater than 50. In an embodiment,a sunblock has a sun protection factor of less than 5, less than 10,less than 15, less than 20, less than 25, less than 30, less than 35,less than 40, less than 45, or less than 50.

Sun protection factor is a dimensionless quantity known to those ofskill in the art. A sun protection factor, or sun protection rating, isa measure of the fraction of UV rays that reach the skin. For example, asun protection factor of 10 means that 1/10 of the UV rays that causesunburn will reach the skin, thus allowing a person that experiencessunburn after 30 minutes to instead experience sunburn after 300minutes. In an embodiment, the UV rays blocked by the sunscreen orsunblock may be ultraviolet type A (UV-A) radiation with a wavelengthrange of about 320-400 nm, ultraviolet type B (UV-B) radiation with awavelength rage of about 320-290 nm, or ultraviolet type C (UV-C)radiation with a wavelength range of about 290-100 nm.

In an embodiment, the invention includes compositions comprisingsunscreen and sunblock compounds, including organic molecules thatabsorb UV-A, UV-B, and/or UV-C radiation, inorganic particles thatscatter UV-A, UV-B, and/or UV-C radiation, and organic particles thatboth absorb and scatter UV-A, UV-B, and/or UV-C radiation. In anembodiment, sunscreen and sunblock compounds include amiloxate(isopentyl-4-methoxycinnamate), para-aminobenzoic acid, Benzophenone-9(sodium dihydroxy dimethoxy disulfobenzophenone), padimate O(octyldimethyl para-aminobenzoic acid), phenylbenzimidazole sulfonicacid, cinoxate, dioxybenzone, oxybenzone, homosalate, menthylanthranilate, 4-methylbenzylidene camphor, Mexoryl XL (drometrizoletrisiloxane), Neo Heliopan AP (disodium phenyl dibenzimidazoletetrasulfonate), octocrylene, octyl methoxycinnamate, octyl salicylate,sulisobenzone, Tinosorb M (bisoctrizole, methylene bis-benzotriazolyltetramethylbutylphenol), Tinosorb S (bis-ethylhexyloxyphenolmethoxyphenol triazine), Tinsorb A2B (tris-biphenyl triazine), trolaminesalicylate, avobenzone, ecamsule, titanium dioxide, Uvinul T 150 (octyltriazone), Uvinul A Plus (diethylamino hydroxybenzoyl hexyl benzoate),Parsol SLX (dimethico-diethylbenzalmalonate), and zinc oxide.

Cleansers

The present invention may include compositions that may be cleansers.For example, the cleansers of the invention may include stearic acidcleansers (which may contain stearic acid), lauric acid cleansers (whichmay contain lauric acid), and combination cleansers. The cleansers ofthe invention may include one or more cleansing agents. Cleansing agentsinclude fatty acids as described herein, such as lauric acid, stearicacid, myristic acid, and oleic acid, and olive oil. Additional cleansingagents may include one or more of non-ionic surfactants, soaps (e.g.,oils described herein that are combined with a caustic agent, such asNaOH and/or KOH), sodium lauryl sulfate, sodium laureth sulfate,palmitic acid, and ammonium laureth sulfate.

Preparation of Moisturizer Compositions

In an embodiment, the extraction temperature during a method ofpreparing a composition of the present disclosure is greater than 84° C.In an embodiment, the extraction temperature during a method ofpreparing a composition of the present disclosure is less than 100° C.In an embodiment, the extraction temperature during a method ofpreparing a composition of the present disclosure is 84° C. to 100° C.In an embodiment, the extraction temperature during a method ofpreparing a composition of the present disclosure is 84° C. to 94° C. Inan embodiment, the extraction temperature during a method of preparing acomposition of the present disclosure is 94° C. to 100° C.

FIG. 1 is a flow chart showing various embodiments for producing puresilk fibroin-based protein fragments (SPFs) of the present disclosure.It should be understood that not all of the steps illustrated arenecessarily required to fabricate all silk solutions of the presentdisclosure. As illustrated in FIG. 1, step A, cocoons (heat-treated ornon-heat-treated), silk fibers, silk powder or spider silk can be usedas the silk source.

If starting from raw silk cocoons from Bombyx mori, the cocoons can becut into small pieces, for example pieces of approximately equal size,step B1. The raw silk is then extracted and rinsed to remove anysericin, step Cla. This results in substantially sericin free raw silk.In an embodiment, water is heated to a temperature between 84° C. and100° C. (ideally boiling) and then Na₂CO₃ (sodium carbonate) is added tothe boiling water until the Na₂CO₃ is completely dissolved. The raw silkis added to the boiling water/Na₂CO₃ (100° C.) and submerged forapproximately 15-90 minutes, where boiling for a longer time results insmaller silk protein fragments. In an embodiment, the water volumeequals about 0.4×raw silk weight and the Na₂CO₃ volume equals about0.848×raw silk weight. In an embodiment, the water volume equals 0.1×rawsilk weight and the Na₂CO₃ volume is maintained at 2.12 g/L. This isdemonstrated in FIG. 62A and FIG. 62B: silk mass (x-axis) was varied inthe same volume of extraction solution (i.e., the same volume of waterand concentration of Na₂CO₃) achieving sericin removal (substantiallysericin free) as demonstrated by an overall silk mass loss of 26 to 31percent (y-axis). Subsequently, the water dissolved Na₂CO₃ solution isdrained and excess water/Na₂CO₃ is removed from the silk fibroin fibers(e.g., ring out the fibroin extract by hand, spin cycle using a machine,etc.). The resulting silk fibroin extract is rinsed with warm to hotwater to remove any remaining adsorbed sericin or contaminate, typicallyat a temperature range of about 40° C. to about 80° C., changing thevolume of water at least once (repeated for as many times as required).The resulting silk fibroin extract is a substantially sericin-depletedsilk fibroin. In an embodiment, the resulting silk fibroin extract isrinsed with water at a temperature of about 60° C. In an embodiment, thevolume of rinse water for each cycle equals 0.1 L to 0.2 L×raw silkweight. It may be advantageous to agitate, turn or circulate the rinsewater to maximize the rinse effect. After rinsing, excess water isremoved from the extracted silk fibroin fibers (e.g., ring out fibroinextract by hand or using a machine). Alternatively, methods known to oneskilled in the art such as pressure, temperature, or other reagents orcombinations thereof may be used for the purpose of sericin extraction.Alternatively, the silk gland (100% sericin free silk protein) can beremoved directly from a worm. This would result in liquid silk protein,without any alteration of the protein structure, free of sericin.

The extracted fibroin fibers are then allowed to dry completely. FIG. 3is a photograph showing dry extracted silk fibroin. Once dry, theextracted silk fibroin is dissolved using a solvent added to the silkfibroin at a temperature between ambient and boiling, step C1b. In anembodiment, the solvent is a solution of Lithium bromide (LiBr) (boilingfor LiBr is 140° C.). Alternatively, the extracted fibroin fibers arenot dried but wet and placed in the solvent; solvent concentration canthen be varied to achieve similar concentrations as to when adding driedsilk to the solvent. The final concentration of LiBr solvent can rangefrom 0.1M to 9.3M. FIG. 63 is a table summarizing the Molecular Weightsof silk dissolved from different concentrations of Lithium Bromide(LiBr) and from different extraction and dissolution sizes. Completedissolution of the extracted fibroin fibers can be achieved by varyingthe treatment time and temperature along with the concentration ofdissolving solvent. Other solvents may be used including, but notlimited to, phosphate phosphoric acid, calcium nitrate, calcium chloridesolution or other concentrated aqueous solutions of inorganic salts. Toensure complete dissolution, the silk fibers should be fully immersedwithin the already heated solvent solution and then maintained at atemperature ranging from about 60° C. to about 140° C. for 1-168 hrs. Inan embodiment, the silk fibers should be fully immersed within thesolvent solution and then placed into a dry oven at a temperature ofabout 100° C. for about 1 hour.

The temperature at which the silk fibroin extract is added to the LiBrsolution (or vice versa) has an effect on the time required tocompletely dissolve the fibroin and on the resulting molecular weightand polydispersity of the final SPF mixture solution. In an embodiment,silk solvent solution concentration is less than or equal to 20% w/v. Inaddition, agitation during introduction or dissolution may be used tofacilitate dissolution at varying temperatures and concentrations. Thetemperature of the LiBr solution will provide control over the silkprotein fragment mixture molecular weight and polydispersity created. Inan embodiment, a higher temperature will more quickly dissolve the silkoffering enhanced process scalability and mass production of silksolution. In an embodiment, using a LiBr solution heated to atemperature between 80° C.-140° C. reduces the time required in an ovenin order to achieve full dissolution. Varying time and temperature at orabove 60° C. of the dissolution solvent will alter and control the MWand polydispersity of the SPF mixture solutions formed from the originalmolecular weight of the native silk fibroin protein.

Alternatively, whole cocoons may be placed directly into a solvent, suchas LiBr, bypassing extraction, step B2. This requires subsequentfiltration of silk worm particles from the silk and solvent solution andsericin removal using methods know in the art for separating hydrophobicand hydrophilic proteins such as a column separation and/orchromatography, ion exchange, chemical precipitation with salt and/orpH, and or enzymatic digestion and filtration or extraction, all methodsare common examples and without limitation for standard proteinseparation methods, step C2. Non-heat treated cocoons with the silkwormremoved, may alternatively be placed into a solvent such as LiBr,bypassing extraction. The methods described above may be used forsericin separation, with the advantage that non-heat treated cocoonswill contain significantly less worm debris.

Dialysis may be used to remove the dissolution solvent from theresulting dissolved fibroin protein fragment solution by dialyzing thesolution against a volume of water, step E1. Pre-filtration prior todialysis is helpful to remove any debris (i.e., silk worm remnants) fromthe silk and LiBr solution, step D. In one example, a 3 μm or 5 μmfilter is used with a flow-rate of 200-300 mL/min to filter a 0.1% to1.0% silk-LiBr solution prior to dialysis and potential concentration ifdesired. A method disclosed herein, as described above, is to use timeand/or temperature to decrease the concentration from 9.3M LiBr to arange from 0.1M to 9.3M to facilitate filtration and downstreamdialysis, particularly when considering creating a scalable processmethod. Alternatively, without the use of additional time or temperate,a 9.3M LiBr-silk protein fragment solution may be diluted with water tofacilitate debris filtration and dialysis. The result of dissolution atthe desired time and temperate filtration is a translucent particle-freeroom temperature shelf-stable silk protein fragment-LiBr solution of aknown MW and polydispersity. It is advantageous to change the dialysiswater regularly until the solvent has been removed (e.g., change waterafter 1 hour, 4 hours, and then every 12 hours for a total of 6 waterchanges). The total number of water volume changes may be varied basedon the resulting concentration of solvent used for silk proteindissolution and fragmentation. After dialysis, the final silk solutionmay be further filtered to remove any remaining debris (i.e., silk wormremnants).

Alternatively, Tangential Flow Filtration (TFF), which is a rapid andefficient method for the separation and purification of biomolecules,may be used to remove the solvent from the resulting dissolved fibroinsolution, step E2. TFF offers a highly pure aqueous silk proteinfragment solution and enables scalability of the process in order toproduce large volumes of the solution in a controlled and repeatablemanner. The silk and LiBr solution may be diluted prior to TFF (20% downto 0.1% silk in either water or LiBr). Pre-filtration as described aboveprior to TFF processing may maintain filter efficiency and potentiallyavoids the creation of silk gel boundary layers on the filter's surfaceas the result of the presence of debris particles. Pre-filtration priorto TFF is also helpful to remove any remaining debris (i.e., silk wormremnants) from the silk and LiBr solution that may cause spontaneous orlong-term gelation of the resulting water only solution, step D. TFF,recirculating or single pass, may be used for the creation of water-silkprotein fragment solutions ranging from 0.1% silk to 30.0% silk (morepreferably, 0.1%-6.0% silk). Different cutoff size TFF membranes may berequired based upon the desired concentration, molecular weight andpolydispersity of the silk protein fragment mixture in solution.Membranes ranging from 1-100 kDa may be necessary for varying molecularweight silk solutions created for example by varying the length ofextraction boil time or the time and temperate in dissolution solvent(e.g., LiBr). In an embodiment, a TFF 5 or 10 kDa membrane is used topurify the silk protein fragment mixture solution and to create thefinal desired silk-to-water ratio. As well, TFF single pass, TFF, andother methods known in the art, such as a falling film evaporator, maybe used to concentrate the solution following removal of the dissolutionsolvent (e.g., LiBr) (with resulting desired concentration ranging from0.1% to 30% silk). This can be used as an alternative to standard HFIPconcentration methods known in the art to create a water-based solution.A larger pore membrane could also be utilized to filter out small silkprotein fragments and to create a solution of higher molecular weightsilk with and/or without tighter polydispersity values. FIG. 61 is atable summarizing Molecular Weights for some embodiments of silk proteinsolutions of the present disclosure. Silk protein solution processingconditions were as follows: 100° C. extraction for 20 min, roomtemperature rinse, Li Br in 60° C. oven for 4-6 hours. TFF processingconditions for water-soluble films were as follows: 100° C. extractionfor 60 min, 60° C. rinse, 100° C. LiBr in 100° C. oven for 60 min. FIGS.67-78 further demonstrate manipulation of extraction time, LiBrdissolution conditions, and TFF processing and resultant examplemolecular weights and polydispersities. These examples are not intendedto be limiting, but rather to demonstrate the potential of specifyingparameters for specific molecular weight silk fragment solutions.

An assay for LiBr and Na₂CO₃ detection was performed using an HPLCsystem equipped with evaporative light scattering detector (ELSD). Thecalculation was performed by linear regression of the resulting peakareas for the analyte plotted against concentration. More than onesample of a number of formulations of the present disclosure was usedfor sample preparation and analysis. Generally, four samples ofdifferent formulations were weighed directly in a 10 mL volumetricflask. The samples were suspended in 5 mL of 20 mM ammonium formate (pH3.0) and kept at 2-8° C. for 2 hours with occasional shaking to extractanalytes from the film. After 2 hours the solution was diluted with 20mM ammonium formate (pH 3.0). The sample solution from the volumetricflask was transferred into HPLC vials and injected into the HPLC-ELSDsystem for the estimation of sodium carbonate and lithium bromide.

The analytical method developed for the quantitation of Na₂CO₃ and LiBrin silk protein formulations was found to be linear in the range 10-165μg/mL, with RSD for injection precision as 2% and 1% for area and 0.38%and 0.19% for retention time for sodium carbonate and lithium bromiderespectively. The analytical method can be applied for the quantitativedetermination of sodium carbonate and lithium bromide in silk proteinformulations.

The final silk protein fragment solution, as shown in FIG. 4, is puresilk protein fragments and water with PPM to undetectable levels ofparticulate debris and/or process contaminants, including LiBr andNa₂CO₃. FIG. 55 and FIG. 58 are tables summarizing LiBr and Na₂CO₃concentrations in solutions of the present disclosure, in FIG. 55, theprocessing conditions included 100° C. extraction for 60 min, 60° C.rinse, 100° C. LiBr in 100° C. oven for 60 min. TFF conditions includingpressure differential and number of dia-filtration volumes were varied.In FIG. 58, the processing conditions included 100° C. boil for 60 min,60° C. rinse, LiBr in 60° C. oven for 4-6 hours. In an embodiment, a SPFcomposition of the present disclosure is not soluble in an aqueoussolution due to the crystallinity of the protein, in an embodiment, aSPF composition of the present disclosure is soluble in an aqueoussolution. In an embodiment, the SPFs of a composition of the presentdisclosure include a crystalline portion of about two-thirds and anamorphous region of about one-third. In an embodiment, the SPFs of acomposition of the present disclosure include a crystalline portion ofabout one-half and an amorphous region of about one-half, in anembodiment, the SPFs of a composition of the present disclosure includea 99% crystalline portion and a 1% amorphous region. In an embodiment,the SPFs of a composition of the present disclosure include a 95%crystalline portion and a 5% amorphous region. In an embodiment, theSPFs of a composition of the present disclosure include a 90%crystalline portion and a 10% amorphous region. In an embodiment, theSPFs of a composition of the present disclosure include an 85%crystalline portion and a 15% amorphous region. In an embodiment, theSPFs of a composition of the present disclosure include an 80%crystalline portion and a 20% amorphous region. In an embodiment, theSPFs of a composition of the present disclosure include a 75%crystalline portion and a 25% amorphous region. In an embodiment, theSPFs of a composition of the present disclosure include a 70%crystalline portion and a 30% amorphous region. In an embodiment, theSPFs of a composition of the present disclosure include a 65%crystalline portion and a 35% amorphous region. In an embodiment, theSPFs of a composition of the present disclosure include a 60%crystalline portion and a 40% amorphous region. In an embodiment, theSPFs of a composition of the present disclosure include a 50%crystalline portion and a 50% amorphous region. In an embodiment, theSPFs of a composition of the present disclosure include a 40%crystalline portion and a 60% amorphous region. In an embodiment, theSPFs of a composition of the present disclosure include a 35%crystalline portion and a 65% amorphous region. In an embodiment, theSPFs of a composition of the present disclosure include a 30%crystalline portion and a 70% amorphous region. In an embodiment, theSPFs of a composition of the present disclosure include a 25%crystalline portion and a 75% amorphous region. In an embodiment, theSPFs of a composition of the present disclosure include a 20%crystalline portion and an 80% amorphous region. In an embodiment, theSPFs of a composition of the present disclosure include a 15%crystalline portion and an 85% amorphous region. In an embodiment, theSPFs of a composition of the present disclosure include a 10%crystalline portion and a 90% amorphous region. In an embodiment, theSPFs of a composition of the present disclosure include a 5% crystallineportion and a 90% amorphous region. In an embodiment, the SPFs of acomposition of the present disclosure include a 1% crystalline portionand a 99% amorphous region.

A unique feature of the SPF compositions of the present disclosure isshelf stability (they will not slowly or spontaneously gel when storedin an aqueous solution and there is no aggregation of fragments andtherefore no increase in molecular weight-over time), from 10 days to 3years depending on storage conditions, percent silk, and number ofshipments and shipment conditions. Additionally pH may be altered toextend shelf-life and/or support shipping conditions by preventingpremature folding and aggregation of the silk. In an embodiment, a SPFsolution composition of the present disclosure has a shelf stability forup to 2 weeks at room temperature (RT). In an embodiment, a SPF solutioncomposition of the present disclosure has a shelf stability for up to 4weeks at RT. In an embodiment, a SPF solution composition of the presentdisclosure has a shelf stability for up to 6 weeks at RT. In anembodiment, a SPF solution composition of the present disclosure has ashelf stability for up to 8 weeks at RT. In an embodiment, a SPFsolution composition of the present disclosure has a shelf stability forup to 10 weeks at RT. In an embodiment, a SPF solution composition ofthe present disclosure has a shelf stability for up to 12 weeks at RT.In an embodiment, a SPF solution composition of the present disclosurehas a shelf stability ranging from about 4 weeks to about 52 weeks atRT. Table 1 below shows shelf stability test results for embodiments ofSPF compositions of the present disclosure.

TABLE 1 Shelf Stability of SPF Compositions of the Present Disclosure %Silk Temperature Time to Gelation 2 RT  4 weeks 2 4 C. >9 weeks 4 RT  4weeks 4 4 C. >9 weeks 6 RT  2 weeks 6 4 C. >9 weeks

A known additive such as a vitamin (e.g., vitamin C, Vitamin B, orVitamin A) can be added to a SPF composition of the present disclosureto create a gel that is stable from 10 days to 3 years at roomtemperature (RT). Both examples, a SPF composition and the same with anadditive, can be lyophilized for enhanced storage control ranging from10 days to 10 years depending on storage and shipment conditions. Thelyophilized silk powder can also be used as a raw ingredient in themedical, consumer, and electronic markets. Additionally, lyophilizedsilk powder can be resuspended in water, HFIP, or organic solutionfollowing storage to create silk solutions of varying concentrations,including higher concentration solutions than those produced initially.In another embodiment, the silk fibroin-based protein fragments aredried using a rototherrn evaporator or other methods known in the artfor creating a dry protein form containing less than 10% water by mass.

Either the silk fragment-water solutions or the lyophilized silk proteinfragment mixture can be sterilized following standard methods in the artnot limited to filtration, heat, radiation or e-beam. It is anticipatedthat the silk protein fragment mixture, because of its shorter proteinpolymer length, will withstand sterilization better than intact silkprotein solutions described in the art. Additionally, silk articlescreated from the SPF mixtures described herein may be sterilized asappropriate to application. For example, a silk film loaded with amolecule to be used in medical applications with an open wound/incision,may be sterilized standard methods such as by radiation or e-beam.

FIG. 2 is a flow chart showing various parameters that can be modifiedduring the process of producing a silk protein fragment solution of thepresent disclosure during the extraction and the dissolution steps.Select method parameters may be altered to achieve distinct finalsolution characteristics depending upon the intended use, e.g.,molecular weight and polydispersity. It should be understood that notall of the steps illustrated are necessarily required to fabricate allsilk solutions of the present disclosure.

In an embodiment, a process for producing a silk protein fragmentsolution of the present disclosure includes forming pieces of silkcocoons from the Bombyx mori silk worm; extracting the pieces at about100° C. in a solution of water and Na₂CO₃ for about 60 minutes, whereina volume of the water equals about 0.4×raw silk weight and the amount ofNa₂CO₃ is about 0.848×the weight of the pieces to form a silk fibroinextract; triple rinsing the silk fibroin extract at about 60° C. forabout 20 minutes per rinse in a volume of rinse water, wherein the rinsewater for each cycle equals about 0.2 L×the weight of the pieces;removing excess water from the silk fibroin extract; drying the silkfibroin extract; dissolving the dry silk fibroin extract in a LiBrsolution, wherein the LiBr solution is first heated to about 100° C. tocreate a silk and LiBr solution and maintained; placing the silk andLiBr solution in a dry oven at about 100° C. for about 60 minutes toachieve complete dissolution and further fragmentation of the nativesilk protein structure into mixture with desired molecular weight andpolydispersity; filtering the solution to remove any remaining debrisfrom the silkworm; diluting the solution with water to result in a 1%silk solution; and removing solvent from the solution using TangentialFlow Filtration (TFF). In an embodiment, a 10 kDa membrane is utilizedto purify the silk solution and create the final desired silk-to-waterratio. TFF can then be used to further concentrate the pure silksolution to a concentration of 2% silk to water.

Each process step from raw cocoons to dialysis is scalable to increaseefficiency in manufacturing. Whole cocoons are currently purchased asthe raw material, but pre-cleaned cocoons or non-heat treated cocoons,where worm removal leaves minimal debris, have also been used. Cuttingand cleaning the cocoons is a manual process, however for scalabilitythis process could be made less labor intensive by, for example, usingan automated machine in combination with compressed air to remove theworm and any particulates, or using a cutting mill to cut the cocoonsinto smaller pieces. The extraction step, currently performed in smallbatches, could be completed in a larger vessel, for example anindustrial washing machine where temperatures at or in between 60° C. to100° C. can be maintained. The rinsing step could also be completed inthe industrial washing machine, eliminating the manual rinse cycles.Dissolution of the silk in LiBr solution could occur in a vessel otherthan a convection oven, for example a stirred tank reactor. Dialyzingthe silk through a series of water changes is a manual and timeintensive process, which could be accelerated by changing certainparameters, for example diluting the silk solution prior to dialysis.The dialysis process could be scaled for manufacturing by usingsemi-automated equipment, for example a tangential flow filtrationsystem.

Varying extraction (i.e., time and temperature), LiBr (i.e., temperatureof LiBr solution when added to silk fibroin extract or vice versa) anddissolution (i.e., time and temperature) parameters results in solventand silk solutions with different viscosities, homogeneities, and colors(see FIGS. 5-32). Increasing the temperature for extraction, lengtheningthe extraction time, using a higher temperature LiBr solution atemersion and over time when dissolving the silk and increasing the timeat temperature (e.g., in an oven as shown here, or an alternative heatsource) all resulted in less viscous and more homogeneous solvent andsilk solutions. While almost all parameters resulted in a viable silksolution, methods that allow complete dissolution to be achieved infewer than 4 to 6 hours are preferred for process scalability.

FIGS. 5-10 show photographs of four different silk extractioncombinations tested: 90° C. 30 min, 90° C. 60 min, 100° C. 30 min, and100° C. 60 min. Briefly, 9.3 M LiBr was prepared and allowed to sit atroom temperature for at least 30 minutes. 5 mL of LiBr solution wasadded to 1.25 g of silk and placed in the 60° C. oven. Samples from eachset were removed at 4, 6, 8, 12, 24, 168 and 192 hours. The remainingsample was photographed.

FIGS. 11-23 show photographs of four different silk extractioncombinations tested: 90° C. 30 min, 90° C. 60 min, 100° C. 30 min, and100° C. 60 min. Briefly, 9.3 M LiBr solution was heated to one of fourtemperatures: 60° C., 80° C., 100° C. or boiling. 5 mL of hot LiBrsolution was added to 1.25 g of silk and placed in the 60° C. oven.Samples from each set were removed at 1, 4 and 6 hours. The remainingsample was photographed.

FIGS. 24-32 show photographs of four different silk extractioncombinations tested: Four different silk extraction combinations wereused: 90° C. 30 min, 90° C. 60 mm, 100° C. 30 min, and 100° C. 60 min.Briefly, 9.3 M LiBr solution was heated to one of four temperatures: 60°C., 80° C., 100° C. or boiling. 5 mL of hot LiBr solution was added to1.25 g of silk and placed in the oven at the same temperature of theLiBr. Samples from each set were removed at 1, 4 and 6 hours. 1 mL ofeach sample was added to 7.5 mL of 9.3 M LiBr and refrigerated forviscosity testing. The remaining sample was photographed.

Molecular weight of the silk protein fragments may be controlled basedupon the specific parameters utilized during the extraction step,including extraction time and temperature; specific parameters utilizedduring the dissolution step, including the LiBr temperature at the timeof submersion of the silk in to the lithium bromide and time that thesolution is maintained at specific temperatures; and specific parametersutilized during the filtration step. By controlling process parametersusing the disclosed methods, it is possible to create SPF mixturesolutions with polydispersity equal to or lower than 2.5 at a variety ofdifferent molecular weight ranging from 5 kDa to 200 kDa, morepreferably between 10 kDa and 80 kDA. By altering process parameters toachieve silk solutions with different molecular weights, a range offragment mixture end products, with desired polydispersity of equal toor less than 2.5 may be targeted based upon the desired performancerequirements. For example, a lower molecular weight silk film containinga drug may have a faster release rate compared to a higher molecularweight film making it more ideal for a daily delivery vehicle inconsumer cosmetics. Additionally, SPF mixture solutions with apolydispersity of greater than 2.5 can be achieved. Further, twosolutions with different average molecular weights and polydispersitiescan be mixed to create combination solutions. Alternatively, a liquidsilk gland (100% sericin free silk protein) that has been removeddirectly from a worm could be used in combination with any of the SPFmixture solutions of the present disclosure. Molecular weight of thepure silk fibroin-based protein fragment composition was determinedusing High Pressure Liquid Chromatography (HPLC) with a Refractive IndexDetector (RID). Polydispersity was calculated using Citrus GPC OnlineGPC/SEC Software Version 3.3 (Agilent).

Parameters were varied during the processing of raw silk cocoons intosilk solution. Varying these parameters affected the MW of the resultingsilk solution. Parameters manipulated included (i) time and temperatureof extraction, (ii) temperature of LiBr, (iii) temperature ofdissolution oven, and (iv) dissolution time. Molecular weight wasdetermined with mass spec as shown in FIGS. 64-80.

Experiments were carried out to determine the effect of varying theextraction time. FIGS. 64-70 are graphs showing these results, andTables 2-8 summarize the results. Below is a summary:

-   -   A sericin extraction time of 30 minutes resulted in larger MW        than a sericin extraction time of 60 minutes    -   MW decreases with time in the oven    -   140° C. LiBr and oven resulted in the low end of the confidence        interval to be below a MW of 9500 Da    -   30 min extraction at the 1 hour and 4 hour time points have        undigested silk    -   30 min extraction at the 1 hour time point resulted in a        significantly high molecular weight with the low end of the        confidence interval being 35,000 Da    -   The range of MW reached for the high end of the confidence        interval was 18000 to 216000 Da (important for offering        solutions with specified upper limit)

TABLE 2 The effect of extraction time (30 min vs 60 min) of molecularweight of silk processed under the conditions of 100° C. ExtractionTemperature, 100° C. Lithium Bromide (LiBr) and 100° C. Oven Dissolution(Oven/Dissolution Time was varied). Boil Oven Average Std ConfidenceTime Time Mw dev Interval PD 30 1 57247 12780 35093 93387 1.63 60 131520 1387 11633 85407 2.71 30 4 40973 2632 14268 117658 2.87 60 4 250821248 10520 59803 2.38 30 6 25604 1405 10252 63943 2.50 60 6 20980 126210073 43695 2.08

TABLE 3 The effect of extraction time (30 min vs 60 min) on molecularweight of silk processed under the conditions of 100° C. ExtractionTemperature, boiling Lithium Bromide (LiBr) and 60° C. Oven Dissolutionfor 4 hr. Boil Average Std Sample Time MW dev Confidence Interval PD 30min, 4 hr 30 49656 4580 17306 142478 2.87 60 min, 4 hr 60 30042 153611183 80705 2.69

TABLE 4 The effect of extraction time (30 min vs 60 min) on molecularweight of silk processed under the conditions of 100° C. ExtractionTemperature, 60° C. Lithium Bromide (LiBr) and 60° C. Oven Dissolution(Oven/ Dissolution Time was varied). Boil Oven Average Std Sample TimeTime MW dev Confidence Interval PD 30 min, 1 hr 30 1 58436 22201 1538092.63 60 min, 1 hr 60 1 31700 11931 84224 2.66 30 min, 4 hr 30 4 61956.513337 21463 178847 2.89 60 min, 4 hr 60 4 25578.5 2446 9979 65564 2.50

TABLE 5 The effect of extraction time (30 min vs 60 min) on molecularweight of silk processed under the conditions of 100° C. ExtractionTemperature, 80° C. Lithium Bromide (LiBr) and 80° C. Oven Dissolutionfor 6 hr. Boil Average Std Confidence Sample Time MW dev Interval PD 30min, 6 hr 30 63510 18693 215775 3.40 60 min, 6 hr 60 25164 238 963765706 2.61

TABLE 6 The effect of extraction time (30 min vs 60 min) on molecularweight of silk processed under the conditions of 100° C. ExtractionTemperature, 80° C. Lithium Bromide (LiBr) and 60° C. Oven Dissolution(Oven/Dissolution Time was varied). Boil Oven Average Std ConfidenceSample Time Time Mw dev Interval PD 30 min, 4 hr 30 4 59202 14028 19073183760 3.10 60 min, 4 hr 60 4 26312.5 637 10266 67442 2.56 30 min, 6 hr30 6 46824 18076 121293 2.59 60 min, 6 hr 60 6 26353 10168 68302 2.59

TABLE 7 The effect of extraction time (30 min vs 60 min) on molecularweight of silk processed under the conditions of 100° C. ExtractionTemperature, 100° C. Lithium Bromide (LiBr) and 60° C. Oven Dissolution(Oven/Dissolution Time was varied). Boil Oven Average Std ConfidenceSample Time Time Mw dev Interval PD 30 min, 4 hr 30 4 47853 19758 1159002.42 60 min, 4 hr 60 4 25082 1248 10520 59804 2.38 30 min, 6 hr 30 655421 8992 19153 160366 2.89 60 min, 6 hr 60 6 20980 1262 10073 436942.08

TABLE 8 The effect of extraction time (30 min vs 60 min) on molecularweight of silk processed under the conditions of 100° C. ExtractionTemperature, 140° C. Lithium Bromide (LiBr) and 140° C. Oven Dissolution(Oven/Dissolution Time was varied). Boil Oven Average Std ConfidenceSample Time Time Mw dev Interval PD 30 min, 4 hr 30 4 9024.5 1102 449318127 2.00865 60 min, 4 hr 60 4 15548 6954 34762 2.2358 30 min, 6 hr 306 13021 5987 28319 2.1749 60 min, 6 hr 60 6 10888 5364 22100 2.0298

Experiments were carried out to determine the effect of varying theextraction temperature. FIG. 71 is a graph showing these results, andTable 9 summarizes the results. Below is a summary:

-   -   Sericin extraction at 90° C. resulted in higher MW than sericin        extraction at 100° C. extraction    -   Both 90° C. and 100° C. show decreasing MW over time in the oven

TABLE 9 The effect of extraction temperature (90° C. vs. 100° C.) onmolecular weight of silk processed under the conditions of 60 min.Extraction Temperature, 100° C. Lithium Bromide (LiBr) and 100° C. OvenDissolution (Oven/Dissolution Time was varied). Boil Oven Average StdConfidence Sample Time Time Mw dev Interval PD 90° C., 4 hr 60 4 373084204 13368 104119 2.79 100° C., 4 hr  60 4 25082 1248 10520 59804 2.3890° C., 6 hr 60 6 34224 1135 12717 92100 2.69 100° C., 6 hr  60 6 209801262 10073 43694 2.08

Experiments were carried out to determine the effect of varying theLithium Bromide (LiBr) temperature when added to silk. FIGS. 72-73 aregraphs showing these results, and Tables 10-11 summarize the results.Below is a summary:

-   -   No impact on MW or confidence interval (all CI-10500-6500 Da)    -   Studies illustrated that the temperature of Li Br-silk        dissolution, as LiBr is added and begins dissolving, rapidly        drops below the original LiBr temperature due to the majority of        the mass being silk at room

TABLE 10 The effect of Lithium Bromide (LiBr) temperature on molecularweight of silk processed under the conditions of 60 min. ExtractionTime., 100° C. Extraction Temperature and 60° C. Oven Dissolution(Oven/Dissolution Time was varied). LiBr Temp Oven Average Sample (° C.)Time Mw Std dev Confidence Interval PD 60 C. LiBr, 1 hr 60 1 31700 1193184223 2.66 100 C. LiBr, 1 hr 100  1 27907 200 10755 72552 2.60 RT LiBr,4 hr RT 4 29217 1082 10789 79119 2.71 60 C. LiBr, 4 hr 60 4 25578 24459978 65564 2.56 80 C. LiBr, 4 hr 80 4 26312 637 10265 67441 2.56 100 C.LiBr, 4 hr 100  4 27681 1729 11279 67931 2.45 Boil LiBr, 4 hr Boil 430042 1535 11183 80704 2.69 RT LiBr, 6 hr RT 6 26543 1893 10783 653322.46 80 C. LiBr, 6 hr 80 6 26353 10167 68301 2.59 100 C. LiBr, 6 hr 100 6 27150 916 11020 66889 2.46

TABLE 11 The effect of Lithium Bromide (LiBr) temperature on molecularweight processed under the conditions of 30 min. Extraction Time, 100°C. Extraction temperature and 60° C. Oven Dissolution (Oven/DissolutionTime was varied). LiBr Temp Oven Average Std Confidence Sample (° C.)Time Mw dev Interval PD 60° C. LiBr, 4 hr 60 4 61956 13336 21463 1788472.89 80° C. LiBr, 4 hr 80 4 59202 14027 19073 183760 3.10 100° C. LiBr,4 hr  100 4 47853 19757 115899 2.42 80° C. LiBr, 6 hr 80 4 47853 18075121292 2.59 100° C. LiBr, 6 hr  100 6 55421 8991 19152 160366 2.89

Experiments were carried out to determine the effect of voven/dissolution temperature. FIGS. 74-78 are graphs showing theseresults, and Tables 12-16 summarize the results. Below is a summary:

-   -   Oven temperature has less of an effect on 60 min extracted silk        than 30 min extracted silk. Without wishing to be bound by        theory, it is believed that the 30 min silk is less degraded        during extraction and therefore the oven temperature has more of        an effect on the larger MW, less degraded portion of the silk.    -   For 60° C. vs. 140° C. oven the 30 min extracted silk showed a        very significant effect of lower MW at higher oven temp, while        60 min extracted silk had an effect but much less    -   The 140° C. oven resulted in a low end in the confidence        interval at ˜6000 Da

TABLE 12 The effect of oven/dissolution temperature on molecular weightof silk processed under the conditions of 100° C. ExtractionTemperature, 30 min. Extraction Time, and 100° C. Lithium Bromide (LiBr)(Oven/Dissolution Time was varied). Oven Boil Temp Oven Average StdConfidence Time (° C.) Time Mw dev Interval PD 30 60 4 47853 19758115900 2.42 30 100 4 40973 2632 14268 117658 2.87 30 60 6 55421 899219153 160366 2.89 30 100 6 25604 1405 10252 63943 2.50

TABLE 13 The effect of oven/dissolution temperature on molecular weightof silk of 100° C. Extraction Temperature, 60 min. Extraction Time, andprocessed under the conditions 100° C. Lithium Bromide (LiBr)Oven/Dissolution Time was varied). Oven Boil Temp Oven Average StdConfidence Time (° C.) Time Mw dev Interval PD 60 60 1 27908 200 1073572552 2.60 60 100 1 31520 1387 11633 85407 2.71 60 60 4 27681 1730 1127972552 2.62 60 100 4 25082 1248 10520 59803 2.38 60 60 6 27150 916 1102066889 2.46 60 100 6 20980 1262 10073 43695 2.08

TABLE 14 The effect of oven/dissolution temperature on molecular weightof silk [processed under the conditions of 100° C. ExtractionTemperature, 60 min. Extraction Time, and 140° C. Lithium Bromide (LiBr)(Oven/Dissolution Time was varied). Oven Boil Temp Oven Average StdConfidence Time (° C.) Time Mw dev Interval PD 60 60 4 30042 1536 1118380705 2.69 60 140 4 15548 7225 33322 2.14

TABLE 15 The effect of oven/dissolution temperature on molecular weightof silk [processed under the conditions of 100° C. ExtractionTemperature, 30 min. Extraction Time, and 140° C. Lithium Bromide LiBr)Oven/Dissolution Time was varied). Oven Boil Temp Oven Average StdConfidence Time (° C.) Time Mw dev Interval PD 30 60 4 49656 4580 17306142478 2.87 30 140 4 9025 1102 4493 18127 2.01 30 60 6 59383 11640 17641199889 3.37 30 140 6 13021 5987 28319 2.17

TABLE 16 The effect of oven/dissolution temperature on molecular weightof silk processed under the conditions of 100° C. ExtractionTemperature, 60 min. Extraction Time, and 80° C. Lithium Bromide (LiBr)(Oven/Dissolution Time was varied). Oven Boil Temp Oven Average StdConfidence Time (° C.) Time Mw dev Interval PD 60 60 4 26313 637 1026667442 2.56 60 80 4 30308 4293 12279 74806 2.47 60 60 6 26353 10168 683022.59 60 80 6 25164 238 9637 65706 2.61

In an embodiment, the methods disclosed herein result in a solution withcharacteristics that can be controlled during manufacturing, including,but not limited to: MW—may be varied by changing extraction and/ordissolution time and temp (e.g., LiBr temperature), pressure, andfiltration (e.g., size exclusion chromatography); Structure—removal orcleavage of heavy or light chain of the fibroin protein polymer;Purity—hot water rinse temperature for improved sericin removal orfilter capability for improved particulate removal that adverselyaffects shelf stability of the silk fragment protein mixture solution;Color—the color of the solution can be controlled with, for example,LiBr temp and time; Viscosity; Clarity; and Stability of solution. Theresultant pH of the solution is typically about 7 and can be alteredusing an acid or base as appropriate to storage requirements.

The above-described SPF mixture solutions may be utilized to produce apure silk protein fragment-film, pure silk protein fragment-gel, or puresilk protein fragment moisturizing composition for numerous applications(e.g., delivery of a drug, vitamin, antioxidant, etc. to the skin). FIG.33 is a flow chart showing an embodiment for producing a silk film ofthe present disclosure from a silk solution of the present disclosure.In step A, a silk solution of the present disclosure is chosen, and thenat least on molecule or therapeutic agent is added directly to the silksolution prior to gel or film processing, step B. When producing a silkfilm, the silk solution with additive(s) may be cast directly onto ashaped mold to achieve a unique film shape (e.g., silicone mold) or thesilk solution may be cast as a sheet and then subsequently cut orpunched into a variety of shapes, with a variety of cutting techniques,including, but not limited to cutting with a rotary blade or lasercutting for example (FIGS. 83A and 83B), depending upon the desiredapplication, step C. If cast on a mold, for example silicone, thesilicone mold may be heated on a laser-etched/patterned surface tocreate an impression that will be transferred to the final film. Forexample, the product logo could be transferred to the film, visible, butnot palpable by hand, and used to show authenticity of the product. Theconcentration and/or mass of the final silk protein fragment film can bevaried to control the film's degree of flexibility and conformity todifferent anatomical topographies. Altering the drying method for a silkfilm will also result in different final film characteristics. Applyingairflow and/or heat impacts the properties of the film (e.g.,brittleness, number of bubbles, curling, solubility, surfaceappearance), step D. Additionally, the percent moisture within the filmat the time of packaging will impact stability over time with too muchmoisture resulting in yellowing of the films with time (FIGS. 82A-82C).In some embodiments, films ideally may have between about 2 to about 20%water content at completion of drying. It was observed that greatermoisture content than 20% in the films will decrease shelf life. Iffilms are not dry enough (that is they have greater than 20% watercontent) before packaging, they will yellow over time (2+ weeks). It isadvised that films are dried in an incubator until the relative humidityin the incubator is less than the relative humidity in the surroundingarea and no greater than 36%. Ambient humidity will have an effect onthe ability to remove moisture and therefore, a tactile/audio test canbe used to determine whether films are ready for packaging. In anembodiment, the test includes removal of a film from the drying system,slightly bending one end of the film and releasing it. If the film feelsand sounds similar to a piece of paper or thin plastic, it is considereddry. If the film has not completed drying, it will be pliable and willmake no noise upon bending and release. In an embodiment, the film isflexible without the need for process additives such as glycerin, suchthat a film that is 2.5 cm wide by 10 cm long can be bent in half sothat opposite ends of the film can touch one another without the filmbreaking or cracking. A film of this same size can be bent in half alongthe length of the film to create a 45-degree angle without breaking orcracking the film.

The final silk protein fragment-film is pure with undetectable levels ofparticulate debris and/or process contaminants, including LiBr andNa₂CO₃. Alternatively, the final SPF mixture solution has less than 500ppm process contaminants. FIG. 56 and FIG. 57 are tables summarizingLiBr and Na₂CO₃ concentrations in films (2% silk films air dried at RT)of the present disclosure. In FIG. 56, the processing conditionsincluded 100° C. extraction for 20 min, RT rinse, LiBr in 60° C. ovenfor 4-6 hours. In FIG. 57, the processing conditions included 100° C.extraction for 20 min, RT rinse, LiBr in 60° C. oven for 4-6 hours.

In an embodiment, when producing a silk gel, an acid is used to helpfacilitate gelation. In an embodiment, when producing a silk gel thatincludes a neutral or a basic molecule and/or therapeutic agent, an acidcan be added to facilitate gelation. In an embodiment, when producing asilk gel, increasing the pH (making the gel more basic) increases theshelf stability of the gel. In an embodiment, when producing a silk gel,increasing the pH (making the gel more basic) allows for a greaterquantity of an acidic molecule to be loaded into the gel.

In an embodiment, natural additives may be added to the silk gel tofurther stabilize additives. For example, trace elements such asselenium or magnesium or L-methionine can be used. Further, light-blockcontainers can be added to further increase stability.

FIG. 34 summarizes an embodiment of parameters for a silk fragment-filmdrying study of the present disclosure. FIG. 35 is a graph showing silkfragment-film drying times (under various air flow and temperatureconditions) based on the silk fragment-film drying study of FIG. 34.These studies indicate that airflow is an important parameter toconsider for drying (i.e., samples in covered containers did not dry),temperature can be altered to alter drying rate (i.e., increasedtemperature results in a faster rate of water removal) and that asteady-state of moisture content within the films can be obtained with avariety of parameters (i.e., from 24 to 48 hours, mass is consistent inuncovered samples regardless of temperature). Of note, the finalproperties of the film, for example brittleness, will vary with dryingconditions. Alternatively, film drying rate may be accelerated by theuse of an additive in the SPF solution, such as a surfactant or oil.These additives may be used with or without heat to alter drying rateand final film physical properties.

In an embodiment, the drying conditions of the SPF film are 24° C. in aforced air flow incubator for 12 to 48 hours depending on the number offilms and ambient humidity. Under these drying conditions, a film thatwill not shrink more than 5 percent over time when stored in a foilpouch is created. Additionally, the film is homogeneous in compositionand physical structure, with no sided-ness and an even distribution ofadditive, for example vitamin C, throughout.

In an embodiment, the silk protein fragment-film may stabilize vitaminC, Vitamin B, Vitamin A, and derivatives thereof at room temperaturewhen stored in light retaining about 30% to about 100% of its activityafter 30 days of storage. In an embodiment, the silk proteinfragment-film may stabilize vitamin C, vitamin B, vitamin A, andderivatives thereof at room temperature when stored in light retainingabout 35% to about 95%) of its activity after 30 days of storage. In anembodiment, the silk protein fragment-film may stabilize vitamin C,vitamin B, vitamin A, and derivatives thereof at room temperature whenstored in light retaining about 40% to about 90% of its activity after30 days of storage. In an embodiment, the silk protein fragment-filmmay-stabilize vitamin C, vitamin B, vitamin A, and derivatives thereofat room temperature when stored in light retaining about 45% to about85% of its activity after 30 days of storage. In an embodiment, the silkprotein fragment-film may stabilize vitamin C, vitamin B, vitamin A, andderivatives thereof at room temperature when stored in light retainingabout 50% to about 80% of its activity after 30 days of storage. In anembodiment, the silk protein fragment-film may stabilize vitamin C,vitamin B, vitamin A, and derivatives thereof at room temperature whenstored in light retaining about 55% to about 75% of its activity after30 days of storage. In an embodiment, the silk protein fragment-film maystabilize vitamin C, vitamin B, vitamin A, and derivatives thereof atroom temperature when stored in light retaining about 60% to about 70%of its activity after 30 days of storage. In an embodiment, the silkprotein fragment-film may stabilize vitamin C, vitamin B, vitamin A, andderivatives thereof at room temperature when stored in a sealed airtightcontainer or pouch that prevents light from contacting the filmretaining about 80% to about 100%) of its activity after 3 to 24 monthsof storage. In an embodiment, the silk protein fragment-film maystabilize vitamin C, vitamin B, vitamin A, and derivatives thereof atroom temperature when stored in a sealed airtight container or pouchthat prevents light from contacting the film retaining about 80% toabout 100% of its activity after about 3 to about 60 months of storage.In an embodiment, the silk protein fragment-film may release between 50%to 90% of active vitamin C, vitamin B, vitamin A, and derivativesthereof within 20 mins when adhered to dampened skin. In an embodiment,the silk protein fragment-film, may release at least 50% active vitaminC, vitamin B, vitamin A, and derivatives thereof within 20 mins whenadhered to dampened skin. In an embodiment, the silk proteinfragment-film may release at least 60% active vitamin C, vitamin B,vitamin A, and derivatives thereof within 20 mins when adhered todampened skin. In an embodiment, the silk protein fragment-film mayrelease at least 70% active vitamin C, vitamin B, vitamin A, andderivatives thereof within 20 mins when adhered to dampened skin. In anembodiment, the silk protein fragment-film may release at least 80%active vitamin C, vitamin B, vitamin A, and derivatives thereof within20 mins when adhered to dampened skin. In an embodiment, the silkprotein fragment-film may release at least 90%) active vitamin C,vitamin B, vitamin A, and derivatives thereof within 20 mins whenadhered to dampened skin. In an embodiment, the silk proteinfragment-film may release between 10% to 100% of active vitamin C,vitamin B, vitamin A, and derivatives thereof within 5 mins to 8 hourswhen adhered to dampened skin. In an embodiment, the silk proteinfragment-film may release at least 10% of active vitamin C, vitamin B,vitamin A, and derivatives thereof within 5 mins to 8 hours when adheredto dampened skin. In an embodiment, the silk protein fragment-film mayrelease at least 20% of active vitamin C, vitamin B, vitamin A, andderivatives thereof within 5 mins to 8 hours when adhered to dampenedskin. In an embodiment, the silk protein fragment-film may release atleast 30% of active vitamin C, vitamin B, vitamin A, and derivativesthereof within 5 mins to 8 hours when adhered to dampened skin. In anembodiment, the silk protein fragment-film may release at least 40% ofactive vitamin C, vitamin B, vitamin A, and derivatives thereof within 5mins to 8 hours when adhered to dampened skin. In an embodiment, thesilk protein fragment-film may release at least 50% of active vitamin C,vitamin B, vitamin A, and derivatives thereof within 5 mins to 8 hourswhen adhered to dampened skin. In an embodiment, the silk proteinfragment-film may release at least 60% of active vitamin C, vitamin B,vitamin A, and derivatives thereof within 5 mins to 8 hours when adheredto dampened skin. In an embodiment, the silk protein fragment-film mayrelease at least 70% of active vitamin C, vitamin B, vitamin A, andderivatives thereof within 5 mins to 8 hours when adhered to dampenedskin. In an embodiment, the silk protein fragment-film may release atleast 80% of active vitamin C, vitamin B, vitamin A, and derivativesthereof within 5 mins to 8 hours when adhered to dampened skin, in anembodiment, the silk protein fragment-film may release at least 90% ofactive vitamin C, vitamin B, vitamin A, and derivatives thereof within 5mins to 8 hours when adhered to dampened skin. It is believed thatexposure to higher temperatures for a longer period of time may breakdown the silk protein into more versatile silk protein fragment mixturesand/or disrupt any silk protein tertiary and/or secondary silk proteinstructure that could adversely affect shelf stability and/or performanceof resulting structures (e.g., moisturizing compositions (e.g. lotions),gels, films, foams, etc.) as well as reduces the number of heavy chainswithin the silk protein.

FIGS. 36A and 36B show two HPLC chromatograms from samples comprisingvitamin C, The chromatogram on the left shows peaks from (1) achemically stabilized sample of vitamin C at ambient conditions and (2)a sample of vitamin C taken after 1 hour at ambient conditions withoutchemical stabilization to prevent oxidation, where degradation productsare visible. The chromatogram on the right shows peaks from twodifferent embodiments of silk films of the present disclosure that wereaged for at least 30 days at room temperature. No degradation productswere visible. FIG. 59 is a table summarizing the vitamin C concentrationin silk protein fragment-films (2% silk films air dried at RT) of thepresent disclosure. In FIG. 59 processing conditions included 100° C.extraction for 20 min, RT rinse, LiBr in 60° C. oven for 4-6 hours, FIG.60 is a table summarizing the stability of vitamin C in chemicallystabilized solutions. FIGS. 89A-89B are tables summarizing vitamin Cstability in SPF gels without chemical stabilizers as compared tochemically stabilized vitamin C in competitive anti-aging skincareproducts. A gel cast at 20% total vitamin C additive concentration didnot gel. Without wishing to be bound by theory, it appears there is arelationship between vitamin C concentration, silk concentration, andgelation. An increase in vitamin C at a given concentration of silk willresult in a longer time to gelation or inhibit gelation. This may be dueto the vitamin C molecule physically blocking interaction between silkprotein fragments or cross-linking of silk protein.

In an embodiment, the molecule or molecules are stable and can bereleased over an extended time period. In an embodiment, release rate iscontrolled by the specific weight average molecular weight of the silkfibroin-based protein fragments used. In another embodiment, releaserate is controlled by creation of a multi-layer structure. For example,multiple films can be cast and dried upon each other. Additionally, eachlayer can be formed using the same or different molecular weightcompositions. In an embodiment, the degree of crystallinity of theprotein structure is altered through film drying conditions, therebycontrolling the release rate. The molecule or molecules may be releasedtopically on the skin, subcutaneously following implantation, or locallyor systemically through oral administration or implantation. In anembodiment, the molecule or molecules is released between 1 minutes and20 minutes. In an embodiment, the molecule or molecules is releasedbetween 20 minutes and 60 minutes, in an embodiment, the molecule ormolecules is released between 1 hour and 4 hours. In an embodiment, themolecule or molecules is released between 4 hours and 8 hours. In anembodiment, the molecule or molecules is released between 8 hours and 24hours. In an embodiment, the molecule or molecules is released between 1day and 7 days. In an embodiment, the molecule or molecules is releasedbetween 1 week and 4 weeks. In an embodiment, the molecule or moleculesis released between 1 month and 3 months. In an embodiment, the moleculeor molecules is released between 3 months and 6 months. In anembodiment, the molecule or molecules is released between 20 minutes and6 months. In an embodiment, the molecule or molecules are stable atextreme temperature and humidity conditions.

Films of the present disclosure comprised of about 20 kDA average weightaverage molecular weight silk fibroin-based protein fragments andcontaining about 20% vitamin C by mass, were stored individually withinfoil pouches and exposed to temperature extremes. Foil pouchescontaining films were exposed to:

-   -   Ambient conditions (time 0 films)    -   “Extreme Cold” (−29° C.±2° C. for 72 hours), followed by “Hot        Humid” (38° C.±2° C. at 85% Humidity±5% for 72 hours), and        subsequently “Extreme Heat, Moderate Humidity” (60° C.±2° C. at        30% Humidity±5% for 6 hours)

The amount of active vitamin C was measured using HPLC. All films wereobserved to support maintenance of vitamin C activity with exposure toextremes, as summarized in Table 17.

TABLE 17 Amount of active vitamin C in films under varying conditionsAverage Conc of vit C N Conditions in sample (mg/g) Std. Dev. 4 Time 0,ambient conditions 184.9 15.15

FIGS. 37-45 are photographs showing silk protein fragment-films of thepresent disclosure dried under various temperature, time and dryingconditions.

FIGS. 46-54 are photographs showing the dissolution, in water, of theformed silk protein fragment-films of the present disclosure undervarious temperature, time and drying conditions. The water solubility offilms of the present disclosure may be varied by altering dryingconditions. For example, drying a film to 20% humidity in a forced airincubator and then increasing ambient humidity to 50% for a period ofhours and subsequently drying the film back to 20% humidity will resultin an insoluble film. Under ordinary conditions where the humidity issteadily decreased, a water-soluble silk film is created. It isanticipated that the increase in humidity allowed the protein structureto be further mobilized in the film and further crystallized, resultingin a non-soluble film. Alternative methods in the art to createnon-soluble films include the introduction of methanol. The films of thepresent disclosure are clearly differentiated from those films due totheir solubility in water. The SPF gel articles described herein rangefrom a hydrogel which can be injected or spread topically to a film-gelarticle that appears as a film and contains a minimal but controlledwater content, thereby preventing crystallinity and allowing watersolubility.

Emulsion Stability

Emulsion stability can be determined by any of the methods known tothose of ordinary skill in the art. In an embodiment, emulsion stabilityis determined by visual analysis of a composition of the presentinvention. In an embodiment, emulsion stability is determined by visualanalysis of a composition of the present invention, wherein the visualanalysis observes phase separation, flocculation, disproportionation,creaming, or instability of an emulsion of the present invention. In anembodiment, emulsion stability is determined by visual analysis of acomposition of the present invention, wherein the visual analysisobserves a change in color. In an embodiment, emulsion stability isdetermined by visual analysis, wherein the visual analysis observes achange in homogeneity of a composition.

In an embodiment, emulsion stability is determined by image analysis ofa composition of the present invention. In an embodiment, emulsionstability is determined by image analysis of a composition of thepresent invention, wherein the image analysis observes phase separation,flocculation, disproportionation, creaming, or instability of anemulsion of the present invention. In an embodiment, emulsion stabilityis determined by image analysis of a composition of the presentinvention, wherein the image analysis observes a change in color of acomposition. In an embodiment, emulsion stability is determined by imageanalysis, wherein the image analysis observes a change in homogeneity ofa composition. In any of the foregoing embodiments, the image analysismay be performed using a microscopic image analysis system. In any ofthe foregoing embodiments, the image analysis may perform a quantitativecolorimetric measurement.

In an embodiment, emulsion stability is determined by turbidity orturbidity ratio analysis of a composition of the present invention.Turbidity and turbidity ratio measurements suitable for analysis ofemulsion stability are known to those of skill in the art and aredescribed, e.g., in Frentcel, et al., J. Disp. Sci. & Tech. 1982, 3,195-207; Song, et al., J. Colloid Interface Sci. 2000, 230, 213-215; andReddy and Fogler, J. Colloid Interface Sci. 1981, 79, 101-104. Turbidityratio methods that compare turbidity at two wavelengths (e.g., 450 nmand 850 nm) may also be used to evaluate emulsion stability. In anembodiment, turbidity is measured with a turbidity meter, such as theAquaLytic AL250T-IR (infrared light), AL400T-WL (white light), orAL450T-IR, or a Hach 2100 Lab Turb. In an embodiment, turbidity ismeasured at 1000 nm, 900 nm, 800 nm, 700 nm, 600 nm, 500 nm, or 400 nm.In an embodiment, turbidity may be measured at an angle of 90° (using anephelometer), with results reported in Nephelometric Turbidity Units.In an embodiment, the turbidity is measured using transmitted light,optionally after calibration with a formazine solution (referencestandard) with results reported in FNUs (Formazine Nephelometric Units).In an embodiment, the turbidity of a composition of the presentinvention remains within 1%, 2%, 5%, 10%, 20%, 30%, 40%, or 50% of itsinitial value at any of the timepoints described herein.

In an embodiment, emulsion stability is determined by emulsion dropletsize distribution analysis of a composition of the present invention. Inan embodiment, emulsion stability is determined by emulsion droplet sizedistribution analysis of a composition of the present invention usinglaser diffraction. In an embodiment, a stable emulsion of the presentinvention exhibits a stable droplet size distribution as determined byemulsion droplet size distribution analysis using laser diffraction. Inan embodiment, a droplet size distribution is determined by one or moreof the following statistics: d10, d50, and d90 (where d10 is thediameter at which 10% of the sample's mass is comprised of smallerdiameter particles, d50 is the diameter at which 50% of the sample'smass is comprised of smaller diameter particles, and d90 is the diameterat which 90% of the sample's mass is comprised of smaller diameterparticles). In an embodiment, a stable emulsion has a d10 selected fromthe group consisting of about 0.1 μm, about 0.5 μm, about 1 μm, about 2μm, about 5 μm, about 10 μm, about 20 μm, about 30 μm, about 40 μm,about 50 μm, and about 100 μm. In an embodiment, a stable emulsion has ad50 selected from the group consisting of about 0.1 μm, about 0.5 μm,about 1 μm, about 2 μm, about 5 μm, about 10 μm, about 20 μm, about 30μm, about 40 μm, about 50 μm, and about 100 μm. In an embodiment, astable emulsion has a d90 selected from the group consisting of about0.1 μm, about 0.5 μm, about 1 μm, about 2 μm, about 5 μm, about 10 μm,about 20 μm, about 30 μm, about 40 μm, about 50 μm, and about 100 μm. Inan embodiment, a stable emulsion has a d10 range selected from the groupconsisting of 0.01 μm to 0.1 μm, 0.1 μm to 1 μm, 1 μm to 2 μm, 2 μm to 5μm, 5 μm to 10 μm, 10 μm to 20 μm, 20 μm to 30 μm, 30 μm to 40 μm, 40 μmto 50 μm, 50 μm to 100 μm, and 100 μm to 200 μm. In an embodiment, astable emulsion has a d50 range selected from the group consisting of0.01 μm to 0.1 μm, 0.1 μm to 1 μm, 1 μm to 2 μm, 2 μm to 5 μm, 5 μm to10 μm, 10 μm to 20 μm, 20 μm to 30 μm, 30 μm to 40 μm, 40 μm to 50 μm,50 μm to 100 μm, and 100 μm to 200 μm. In an embodiment, a stableemulsion has a d90 range selected from the group consisting of 0.01 μmto 0.1 μm, 0.1 μm to 1 μm, 1 μm to 2 μm, 2 μm to 5 μm, 5 μm to 10 μm, 10μm to 20 μm, 20 μm to 30 μm, 30 μm to 40 μm, 40 μm to 50 μm, 50 μm to100 μm, and 100 μm to 200 μm. In an embodiment, the d10, d50, or d90 ofa composition of the present invention remains within 1%, 2%, 5%, 10%,20%, 30%, 40%, or 50% of its initial value at any of the timepointsdescribed herein.

In an embodiment, emulsion stability is determined by pH measurement. Inan embodiment, emulsion stability is determined by viscosity using arotational viscometer. In an embodiment, emulsion stability isdetermined by oscillatory shear viscosity using a rheometer. In anembodiment, emulsion stability is determined by organoleptic analysis.In an embodiment, emulsion stability is determined by measuring specificgravity using a pycnometer. In an embodiment, emulsion stability isdetermined by measuring conductivity using a conductivity meter. In anembodiment, emulsion stability of a composition of the present inventionmeasured by any of the foregoing methods remains within 1%, 2%, 5%, 10%,20%, 30%, 40%, or 50% of its initial value at any of the timepointsdescribed herein.

In an embodiment, emulsion stability is determined at time points duringstorage at ambient temperature. In an embodiment, emulsion stability isdetermined after storage at 25° C. for 1 day, 2 days, 3 days, 4 days, 5days, 6, days, 1 week, 2 weeks, 3 weeks, 1 month, 1.5 months, 2 months,2.5 months, 3 months, 4 months, 5 months, 6 months, 7 months, 8 months,9 months, 10 months, 11 months, 1 year, 1.5 years, 2 years, 2.5 years, 3years, 4 years, or 5 years. In an embodiment, emulsion stability isdetermined after storage at 30° C. for 1 day, 2 days, 3 days, 4 days, 5days, 6, days, 1 week, 2 weeks, 3 weeks, 1 month, 1.5 months, 2 months,2.5 months, 3 months, 4 months, 5 months, 6 months, 7 months, 8 months,9 months, 10 months, 11 months, 1 year, 1.5 years, 2 years, 2.5 years, 3years, 4 years, or 5 years. In an embodiment, emulsion stability isdetermined after storage at 37° C. for 1 day, 2 days, 3 days, 4 days, 5days, 6, days, 1 week, 2 weeks, 3 weeks, 1 month, 1.5 months, 2 months,2.5 months, 3 months, 4 months, 5 months, 6 months, 7 months, 8 months,9 months, 10 months, 11 months, 1 year, 1.5 years, 2 years, 2.5 years, 3years, 4 years, or 5 years. In an embodiment, emulsion stability isdetermined after storage at 45° C. for 1 day, 2 days, 3 days, 4 days, 5days, 6, days, 1 week, 2 weeks, 3 weeks, 1 month, 1.5 months, 2 months,2.5 months, 3 months, 4 months, 5 months, 6 months, 7 months, 8 months,9 months, 10 months, 11 months, 1 year, 1.5 years, 2 years, 2.5 years, 3years, 4 years, or 5 years. In an embodiment, emulsion stability isdetermined after storage at 4° C. for 1 day, 2 days, 3 days, 4 days, 5days, 6, days, 1 week, 2 weeks, 3 weeks, 1 month, 1.5 months, 2 months,2.5 months, 3 months, 4 months, 5 months, 6 months, 7 months, 8 months,9 months, 10 months, 11 months, 1 year, 1.5 years, 2 years, 2.5 years, 3years, 4 years, or 5 years. In an embodiment, emulsion stability isdetermined after storage at −10° C. for 1 day, 2 days, 3 days, 4 days, 5days, 6, days, 1 week, 2 weeks, 3 weeks, 1 month, 1.5 months, 2 months,2.5 months, 3 months, 4 months, 5 months, 6 months, 7 months, 8 months,9 months, 10 months, 11 months, 1 year, 1.5 years, 2 years, 2.5 years, 3years, 4 years, or 5 years. In an embodiment, emulsion stability isdetermined after storage at in a cycling chamber, which cycles between4° C. and 45° C. over 48 hours, for 1 day, 2 days, 3 days, 4 days, 5days, 6, days, 1 week, 2 weeks, 3 weeks, 1 month, 1.5 months, 2 months,2.5 months, 3 months, 4 months, 5 months, 6 months, 7 months, 8 months,9 months, 10 months, 11 months, 1 year, 1.5 years, 2 years, 2.5 years, 3years, 4 years, or 5 years. In an embodiment, emulsion stability isdetermined after storage at on a shaker table, for 1 day, 2 days, 3days, 4 days, 5 days, 6, days, 1 week, 2 weeks, 3 weeks, 1 month, 1.5months, 2 months, 2.5 months, 3 months, 4 months, 5 months, 6 months, 7months, 8 months, 9 months, 10 months, 11 months, 1 year, 1.5 years, 2years, 2.5 years, 3 years, 4 years, or 5 years.

The following examples are put forth so as to provide those of ordinaryskill in the art with a complete disclosure and description of how tomake and use the described embodiments, and are not intended to limitthe scope of what the inventors regard as their invention nor are theyintended to represent that the experiments below are all or the onlyexperiments performed. Efforts have been made to ensure accuracy with,respect to numbers used (e.g. amounts, temperature, etc.) but someexperimental errors and deviations should be accounted for. Unlessindicated otherwise, parts are parts by weight, molecular weight isweight average molecular weight, temperature is in degrees Centigrade,and pressure is at or near atmospheric.

EXAMPLES Example 1. Development of a Silk Film of the Present Disclosurefor Use in Fine Line Lifting Applications

TABLE 18 Film Recipe for Fine Line Lifting Film - FIG. 82A % SPF MixtureSolution of the 2.4% Present Disclosure Quantity Vitamin C 4:1 (silk:VitC) (0.006 g/mL 2.4% solution) 20% mL per film (2.5 cm by 10 cm) 7.08 mLMass of silk per film:  170 mg Mass of I-ascorbic acid per film: 42.5 mgpH 4.0 (when water is applied)

Silk films (2.5 cm×10 cm) were manufactured according to methodsdisclosed herein varying process parameters so as to result in fine linelifting films. The silk films were given the name “PureProC™ film,” andcan be packaged in a foil based package that is air tight and lightproof. Table 18 provides details of the PureProC™ films used in a studyof 32 individuals using the films for four (4) weeks. Biocompatibilityand hypo-allergenicity of the films was observed. Further, nosensitization, toxicity, or immune response was observed. FIG. 84 is agraph summarizing the quantity of vitamin C in a daily dose (i.e., theaverage amount of product used to cover a 25 cm² area of skin) ofPureProC™ and competitor products over a 30 day period. FIGS. 85 and 86summarize resultant ease of use data and observed benefits within thefirst month of use.

In an embodiment, PureProC™ films were removed by peeling the films off.In an embodiment, PureProC™ films were removed by using a wet cottonball or similar removal pad. In an embodiment, PureProC™ films wereremoved by washing the area where the film is placed with a wash cloth.In an embodiment, PureProC™ film PureProC™ films were removed usingwater. The PureProC™ films can be shaped into strips for multiple areasof the face or larger pieces can be cut to fit target areas. In anembodiment, grips or backing(s) on the PureProC™ films can be includedfor ease of application. In an embodiment, a PureProC™ film of thepresent disclosure includes silk and vitamin C (20%).

In an embodiment, a film of the present disclosure is soluble in water(insoluble border). In an embodiment, a film of the present disclosureis clear/transparent. In an embodiment, a film of the present disclosurehas a pH=4 when water is applied. Films of the present disclosure can bemade with different combinations of % silk and volume to produce filmswith silk quantities of 3 mg/cm² to 10 mg/cm². Films of the presentdisclosure can be made with from about 1% to about 50% 1-ascorbic acid.Films of the present disclosure can adhere to skin with water. Films ofthe present disclosure can be spread on skin once water is applied.Films of the present disclosure can dry when humidity of dryingequipment is 16-40% and below the humidity of the lab.

Example 2. Development of Silk Gels of the Present Disclosure

TABLE 19 Gel Samples-Silk gel formulations including additives,concentration of silk and additive, gelation conditions and gelationtimes. mL 2% Mass Ratio Amount Sample silk Vit C Silk: of Temp/ Days toName solution (g) Vit C Additive additive treatment Gelation 1 10 0.045:01 None None RT 8 2 10 0.08 2.5:1   None None RT 8 3 10 0.2 1:01 NoneNone RT 8 4 10 0.4 1:02 None None RT 14 5 10 0.8 1:04 None None RT None6 10 0.04 5:01 None None RT ~39 7 10 0.08 2.5:1    None None Fridge ~398 10 0.2 1:01 None None Fridge ~39 9 10 0.4 1:02 None None Fridge None10 10 0.8 1:04 None None Fridge None 11 10 0.2 1:01 None None RT/Shake 8vigorously O-1 10 0.04 5:01 None None 37° C. Oven 3 O-2 10 0.04 5:01None None 50° C. Oven 2 O-3 10 0.02 1:01 None None 37° C. Oven 4 O-4 100.02 1:01 None None 50° C. Oven 3 M 40 0.16 5:01 None None RT 5 D 400.16 5:01 None None RT 5 E1 10 0.04 5:01 Vit E 1 drop RT 7 E2 10 0.045:01 Vit E  3 drops RT 7 E3 10 0 None Vit E 1 drop RT None E4 10 0 NoneVit E 3 drops RT None L1 10 0.04 5:01 Lemon 300 uL RT 6 L2 10 0.04 5:01Lemon 300 uL RT 6 juice L3 10 0.04 5:01 Lemon 1000 uL RT 5 juice L4 10 00 Lemon 300 uL RT 6 L5 10 0 0 Lemon 300 uL RT 7 juice Jar 1 20 0.08 5:01Lemon 2000 uL RT 5-7 juice Jar 2 5 0.02 5:01 Lemongrass 1 drop RT 2-3oil R-1 10 0.04 5:01 Rosemary 1 drop RT 7 Oil T-1 10 0.04 5:01 None NoneRT/Tube 7 RO-1 10 0.04 5:01 Rose Oil 1 drop RT 6 RO-2 10 None None RoseOil 1 drop RT None

Ratio of Silk to Vitamin C

Samples 1-10 were used to examine the effect of silk to vitamin C ratioon serum gelation. Samples 1-3 with less vitamin C gelled quicker thansamples 4 and 5. All other conditions were kept constant. Samples 6-8with less vitamin C gelled quicker than samples 9 and 10. All otherconditions were kept constant. It is concluded that decreasing the ratioof silk to vitamin C (increasing the amount of vitamin C) will lengthenthe time to gel creation. At ratios with small amounts of vitamin C,days to gel creation did not vary greatly.

Physical Stimulation

Samples 3 and 11 were used to examine the effect of physical stimulationon serum gelation. Each sample was prepared under the same conditions.Sample 11 was vigorously shaken for about 3 minutes after addition ofvitamin C. Treatment of 3 and 11 was otherwise the same. The shakingresulted in bubbles but did not significantly change gel creation time.

Temperature Treatment

Samples 1, 3, 6, 8, 0-1, 0-2, 0-3, and 0-4 were used to examine theeffect of temperature treatment on serum gelation time. Samples 1, 6,0-1, and 0-2 were identical other than temperature treatment. Samples 3,8, 0-3, and 0-4 were identical other than temperature treatment. The twogroups differed in silk to vitamin C ratio. Time to serum gelation wasdirectly related to temperature treatment with a higher temperatureresulting in quicker serum gelation.

Solution Volume

Samples 1, M and D were used to examine the effect of solution volume onserum gelation time. Samples M and D varied from sample 1 only by anincreased solution volume. Samples M and D gelled in 5 days while sample1 gelled in 8 days. Samples M and D were definitively noticed to begelled on the day of gelling while sample 1 gelled over a weekend.

Additives

Samples E1, E2, E3, E4, L1, L2, L3, L4, L5, Jar 2, R1, RO-1 and RO-2were used to examine the effect of additives on serum gelation time.Samples E1-4 contained Vitamin E. Only samples E1 and E2 containedvitamin C and only these two samples gelled. Vitamin E can be added to asolution to become a gel but it appears that another additive may beneeded to create a gel. Samples L1-5 contained a form of lemon juice.Samples L1 and L4 had juice directly from a lemon while samples L2, L3and L5 contained lemon juice from a plastic lemon container. Samples L4and L5 did not have vitamin C while all others did. All samples gelledshowing that lemon juice can create gel on its own. Amount of lemonjuice and type of lemon juice had little effect on gelation time. SampleJar 2 contained lemon grass oil which formed an albumen like substancewhen initially added. This sample also had vitamin C but gelation timewas significantly quicker than with other vitamin C samples. Sample R1contained rosemary oil, which seemed to be soluble, as well as vitaminC. The sample gelled in a similar time frame to other samples with onlyvitamin C. Samples RO-1 and RO-2 contained rose oil while only RO-1 hadvitamin C. Only RO-1 gelled showing that rose oil will not create a gelquickly on its own. In both cases the rose oil was immiscible andvisible as yellow bubbles.

Aqueous silk fibroin-based fragment solution and essential oils areimmiscible liquids. In an embodiment, to increase the fragrance of thesilk fibroin-based fragment solution, without entrapping oils within thesolution, the solution is mixed with the essential oil with the use of astir bar. The stir bar is rotated at a speed such that some turbulenceis observed in the mixture, thus causing contact between the fragrantessential oil and the molecules in solution, adding a scent to thesolution. Before casting of product from the solution, mixing may bestopped and the oil allowed to separate to the top of the solution.Dispensing from the bottom fraction of the solution into the finalproduct allows for fragrance without visible essential oil within thefinal product.

Alternatively, the silk fibroin-based solution and essential oil can becombined with or without additional ingredients and/or an emulsifier tocreate a composition containing both ingredients.

In an embodiment, mixing of the solution as described above can reducegelation time if the solution is used to create a gel formulation.

Vessel

Samples T1 and Jar 1 were used to examine the effect of casting vesselon serum gelation time. Jar 1 was cast in a glass jar while T1 was castin an aluminum tube. Both samples gelled and did not affect serum geltime.

SUMMARY

All treatments of silk solution for gel solution were in a conical tubeat room temperature unless otherwise stated. The ratio of silk tovitamin C did affect the ability of a solution to gel as ratios above1:2 did not gel and a 1:2 ratio took twice as long as other lower ratios(5:1, 2.5:1, 1:1). Temperature affected gel creation time with highertemperatures resulting in quicker gel times. 50° C. treatment gelled inas quick as 2 days, 37° C. treatment gelled in as quick as 3 days, roomtemperature treatment gelled in 5-8 days and storage in a refrigeratortook at least 39 days to gel.

The effects of additives on gel creation were dependent on the additive.Vitamin E, Rosemary Oil and Rose Oil all had no effect on gel creation.Each of these additives did not prevent gelation or affect the time togelation. Each also required the presence of vitamin C to gel. Lemonjuice from a fresh lemon, pre-squeezed lemon juice from a plastic lemoncontainer and lemon grass oil did affect gel creation. Without wishingto be bound by theory, it is believed that the lower pH as a result ofthese additives is the reason the additives had an impact on decreasinggelation time. Both lemon juice types were able to cause gelationwithout the presence of vitamin C. This occurred in the same number ofdays as with vitamin C. The lemongrass oil was able to decrease thenumber of days to gelation to 2-3 days. Ail additives appeared solubleother than lemongrass oil and rose oil. Rose oil remained in yellowbubbles while the lemongrass oil was partially soluble and formed analbumen like chunk. In an embodiment, oils that are not fully solublecan still be suspended within the gel as an additive. Physicalstimulation by shaking, vessel the solution was cast into and solutionvolume did not affect gelation time. FIG. 81 is a graph representing the% Activity of Vitamin C in gels of the present disclosure.

TABLE 20 Concentration of vitamin C in various gel formulations. SampleConcentration of Weight Vitamin C (mg/g) Sample Info (mg) In SampleAverage Rosemary 685.7 3.2511 3.2657 (Room 3.2804 Temperature 638 3.33363.3334 storage) 3.3332 Lemongrass 646 2.8672 2.877 (Room 2.8868Temperature 645.5 2.9051 2.9051 storage) 2.9052 Rosemary 645.2 3.90633.9147 (Room 3.923 Temperature; 649 3.9443 3.9374 Foil Covered 3.9305storage) Lemongrass 630.1 3.8253 3.8274

TABLE 20 Concentration of vitamin C in various gel formulations SampleConcentration Weight of Vitamin C (mg/g) Sample Info (mg) In SampleAverage Rosemary (Room 685.7 3.2511 3.2657 Temperature storage) 3.2804638 3.3336 3.3334 3.3332 Lemongrass (Room 646 2.8672 2.877 Temperaturestorage) 2.8868 645.5 2.9051 2.9052 2.9052 Rosemary (Room 645.2 3.90633.9147 Temperature; Foil 3.923 Covered storage) 649 3.9443 3.9374 3.9305Lemongrass (Room 630.1 3.9443 3.9374 Temperature; Foil 3.9305 Coveredstorage) 660.4 3.8253 3.8274 3.8295 Rosemary (Fridge, Foil 672.4 5.16165.1484 Covered storage) 5.1352 616.5 5.1984 5.201 5.2036 Lemongrass(Fridge, 640.5 5.1871 5.1824 Foil Covered storage) 5.1776 627.7 5.20985.2126 5.2154

Example 3. Development of Silk Gels of the Present Disclosure for Use asSmoothing

TABLE 21 Lemongrass Gel % Silk Solution 2% Quantity Vitamin C 100 mg/15mL solution Quantity Lemongrass Oil 20 uL/15 mL solution

TABLE 22 Rosemary Gel % Silk Solution 2% Quantity Vitamin C 100 mg/15 mLsolution Quantity Rosemary Oil 20 uL/50 mL solution

TABLE 23 Lemongrass Gel (50 mL) % Silk Solution (60 minute boil, 25 kDA)2% Quantity Vitamin C (ascorbyl glucoside) 12.82 mg/mL solution (641 mgtotal) Quantity Lemongrass Oil 1.33 uL/mL solution pH 4

TABLE 24 Rosemary Gel (50 mL) % Silk Solution (60 minute boil, 25 kDA)2% Quantity Vitamin C (ascorbyl glucoside) 12.82 mg/mL solution (641 mgtotal) Quantity Rosemary Oil 0.8 uL/mL solution pH 4

Gels of the present disclosure can be made with about 0.5% to about 8%silk solutions. Gels of the present disclosure can be made with ascorbylglucoside at concentrations of about 0.67% to about 15% w/v. Gels of thepresent disclosure be clear/white in color. Gels of the presentdisclosure can have a consistency that is easily spread and absorbed bythe skin. Gels of the present disclosure can produce no visual residueor oily feel after application. Gels of the present disclosure do notbrown over time.

Silk gels with essential oils were prepared by diluting a silk solutionof the present disclosure to 2%. Vitamin C was added to the solution andallowed to dissolve. The essential oil was added, stirred and dissolved.The solution was aliquot into jars.

A trial was conducted with 44 people on two formulations of the presentdisclosure, PureProC™ Rosemary Gel and PureProC™ Lemongrass Gel (FIGS.87 and 88). Respondents were asked to use each sample once a day for aweek each. The majority of respondents applied the gel to the wholeface. Other areas where it was most commonly applied included theforehead, under eyes and near mouth.

The majority of respondents applied the gel during the morning (67%)with the balance 33% applying the gel in the evening. Ninety-eight (98%)of participants used the gel once a day during the test. Respondentswere asked to describe in their own words how the gel felt when it wasapplied and how it felt during the 24 hours until the next application.Smooth, cool, and soft were the most often mentioned adjectives used todescribe how the gel felt. Eighty percent (80%) of test participantsgave a high score to interest in continuing to use the gel.

Respondents were asked about what they did with their other productsthat were usually used on their face during the trial. The majorityapplied the gel first and then added the other products or applied thegel at night with no additional products. Only 14% of participantsindicated that they eliminated one of their normal products whiletesting the gel. PureProC™ can be used in conjunction with or inreplacement of other products. Additionally, sunscreen can be added tothe gel or it may be dispensed from a pump instead of a jar. Withrepeated topical use, no skin irritation, rash, or signs ofnon-compatibility was observed. Biocompatibility and hypo-allergenicityof the gels was observed. Further, no sensitization, toxicity, or immuneresponse was observed.

Example 4. Silk Articles of the Present Disclosure Made From SilkSolutions of the Present Disclosure

Silk solutions of various molecular weights and/or combinations ofmolecular weights can be optimized for specific applications. Thefollowing provides an example of this process but it not intended to belimiting in application or formulation.

Three (3) silk solutions were utilized in standard silk structures inaccordance with standard methods in the literature with the followingresults:

-   -   Solution #1 is a silk concentration of 5.9%, average MW of 19.8        kDa and 2.2 PD (made with a 60 min boil extraction, 100 degree        LiBr dissolution for 1 hr)    -   Solution #2 is a silk concentration of 6.4% (made with a 30 min        boil extraction, 60 degree I.iBr dissolution for 4 hrs)    -   Solution #3 is a silk concentration of 6.17% (made with a 30 min        boil extraction, 100 C LiBr dissolution for 1 hour)

Films: Films were made in accordance with Rockwood et al (NatureProtocols; Vol. 6; No. 10; published on-line Sep. 22, 2011; doi:10.1038/nprot.2011.379). Briefly, 4 mL of 1% or 2% (wt/vol) aqueous silksolution was added into 100 mm Petri dish (Volume of silk can be variedfor thicker or thinner films and is not critical) and allowed to dryovernight uncovered. The bottom of a vacuum desiccator was filled withwater. Dry films were placed in the desiccator and vacuum applied,allowing the films to water anneal for 4 hours prior to removal from thedish. Films cast from solution #1 did not result in a structurallycontinuous film; the film was cracked in several pieces. These pieces offilm dissolved in water in spite of the water annealing treatment.

Egel: “Egel” is an electro gelation process as described in Rockwood etal. Briefly, 10 ml of aqueous silk solution is added to a 50 ml conicaltube and a pair of platinum wire electrodes immersed into the silksolution. A 20 volt potential was applied to the platinum electrodes for5 minutes, the power supply turned off and the gel collected. Solution#1 did not form an EGEL over the 5 minutes of applied electric current.

Gelation: Solutions #2 and #3 were gelled in accordance with thepublished horseradish peroxidase (HRP) protocol. Behavior seemed typicalof published solutions.

Sonicated Gels: Gels were made following the sonication process inRockwood et al.

Briefly, 5 ml of silk solution was added to a 15 ml conical tube. Thesonicating horn was immersed in the solution and the solution sonicatedat 50% amplitude (21W). Silk gels were made with 2%, 4% and 6% silksolutions. As compared to standard literature silk, Solutions #2 and #3formed gels after a longer time, for example:

-   -   Standard literature silk: 5-8 min    -   Solution #2; 20 min    -   Solution #3: 120 min

Porous 3D scaffolds: Water based, salt leached scaffolds were made inaccordance with the published methods of Rockwood. Salt with particlesizes of interest was prepared by stacking the sieves with the largestmesh on top and the smallest mesh on the bottom. Salt was added andsieves shaken vigorously collecting the salt. With a 5 ml syringe, 6%(wt/vol) fibroin solution was aliquoted into plastic containers, 2 mlper mold and 5-600 micron salt particles were slowly added on top of thefibroin solution in the mold while rotating the container so that thesalt was uniform. The ratio of salt to silk in solution was maintainedat 25:1

The container was gently tapped on the bench to remove air bubbles, thecap closed and the solution allowed to settle overnight at roomtemperature. Once gelled, the lids were removed and the molds placed ina 2-liter beaker with ultrapure water (three containers per 2 liters ofwater). The beakers were transferred to a stir plate and stirred,changing the water 2-3 times per day for 2 d (4-5 washes in total). Thescaffolds were removed from the molds and placed them in fresh water foran additional day.

Solution #1 did not form a scaffold; it did not gel. Both solution #2 &#3 formed scaffolds. The scaffolds made with Solution #3 appear softerthan the ones made with Solution #2, but both scaffolds werehomogeneous.

Example 5. Tangential Flow Filtration (TFF) to Remove Solvent fromDissolved Silk Solutions of the Present Disclosure

A variety of % silk concentrations have been produced through the use ofTangential Flow Filtration (TFF). In all cases a 1% silk solution wasused as the input feed. A range of 750-18,000 mL of 1% silk solution wasused as the starting volume. Solution is diafiltered in the TFF toremove lithium bromide. Once below a specified level of residual LiBr,solution undergoes ultrafiltration to increase the concentration throughremoval of water. See examples below.

7.30% Silk Solution: A 7.30% silk solution was produced beginning with30 minute extraction batches of 100 g silk cocoons per batch. Extractedsilk fibers were then dissolved using 100 C 9.3M LiBr in a 100 C ovenfor 1 hour. 100 g of silk fibers were dissolved per batch to create 20%silk in LiBr. Dissolved silk in LiBr was then diluted to 1% silk andfiltered through a 5 um filter to remove large debris. 15,500 mL of 1%,filtered silk solution was used as the starting volume/diafiltrationvolume for TFF. Once LiBr was removed, the solution was ultrafiltered toa volume around 1300 mL. 1262 mL of 7.30% silk was then collected. Waterwas added to the feed to help remove the remaining solution and 547 mLof 3.91% silk was then collected.

6.44% Silk Solution: A 6.44% silk solution was produced beginning with60 minute extraction batches of a mix of 25, 33, 50, 75 and 100 g silkcocoons per batch. Extracted silk fibers were then dissolved using 100 C9.3M LiBr in a 100 C oven for 1 hour, 35, 42, 50 and 71 g per batch ofsilk fibers were dissolved to create 20% silk in LiBr and combined.Dissolved silk in LiBr was then diluted to 1% silk and filtered througha 5 um filter to remove large debris. 17,000 mL of 1%, filtered silksolution was used as the starting volume/diafiltration volume for TFF.Once LiBr was removed, the solution was ultrafiltered to a volume around3000 mL. 1490 mL of 6.44% silk was then collected. Water was added tothe feed to help remove the remaining solution and 1454 mL of 4.88%)silk was then collected

2.70% Silk Solution: A 2.70% silk solution was produced beginning with60 minute extraction batches of 25 g silk cocoons per batch. Extractedsilk fibers were then dissolved using 100 C 9.3M LiBr in a 100 C ovenfor 1 hour. 35.48 g of silk fibers were dissolved per batch to create20% silk in LiBr. Dissolved silk in LiBr was then diluted to 1% silk andfiltered through a 5 um filter to remove large debris. 1000 mL of 1%,filtered silk solution was used as the starting volume/diafiltrationvolume for TFF. Once LiBr was removed, the solution was ultrafiltered toa volume around 300 mL. 312 mL of 2.7% silk was then collected.

Example 6. Gel Vitamin C Derivatives of the Present Disclosure

The purest form of vitamin C is L-ascorbic acid. There are a number ofother derivatives of vitamin C that function like pure vitamin C afterthey are converted to L-ascorbic acid in the body. Vitamin C derivativesare being utilized to extend shelf life. Derivatives are stable forms ofL-ascorbic acid and will not oxidize or lose stability. Table 25 belowsummarizes some vitamin C derivatives tested in the skin care productsof the present disclosure:

TABLE 25 Derivatives Explored Sodium Ascorbyl Phosphate (Aromantic)Sodium Ascorbyl Phosphate (DSM) Magnesium Ascorbyl Phosphate AscorbicAcid-2-Glucoside Ascorbyl Tetraisopalmitate

The Tables in FIGS. 89A-89B summarize embodiments of gels of the presentdisclosure. Ascorbic acid-2-glucoside was the most successful vitamin Cderivative at gel formation with gel being formed in a 2% silk solutionin 3 days. Sodium ascorbyl phosphate from DSM supplier formed a gel in a2% silk solution after 28 days while the same molecule from Aromanticfailed to create a gel. In all cases 100 mg of vitamin C derivative wasmixed in 15 mL of 2% silk solution, and all gels had the same appearanceas gels created with ascorbic acid.

Gels were also cast with combinations of two vitamin C options. In eachcase, at least one of the vitamin C options was known to cause gelation(L-ascorbic acid or ascorbic acid-2-glucoside). All combination gelswere able to gel at 1% total vitamin C additive concentration. A gelcast at 20% total vitamin C additive concentration did not gel. Withoutwishing to be bound by theory, it appears there is a relationshipbetween vitamin C concentration, silk concentration, and gelation. Anincrease in vitamin C at a given concentration of silk will result in alonger time to gelation or inhibit gelation. This may be due to thevitamin C molecule physically blocking interaction between silk proteinfragments or cross-linking of silk protein. Modification to pH may allowadditional concentrations of vitamin C and derivatives thereof to beadded.

Ascorbyl tetraisopalmitate was not used in any gel forming formulation,as it was unable to dissolve or be dispersed in an aqueous silksolution. Ascorbyl tetraisopalmitate is a highly viscous, oil solubleliquid that might need the help of an emulsifier to possible dissolve inaqueous silk solution.

Example 7. Film Vitamin C Derivatives of the Present Disclosure

FIG. 90 is a table summarizing embodiments of films of the presentdisclosure. Sodium ascorbyl phosphate, magnesium ascorbyl phosphate andascorbic acid-2-glucoside could be cast in films with varyingappearance. Sodium ascorbyl phosphate films were opaque and white with atextured top surface similar to plastic. Magnesium ascorbyl phosphatefilms were clear and cloudy with a textured top surface similar toplastic. Ascorbic acid-2-glucoside films were most similar to L-ascorbicacid films although slightly less pliable and slightly textured. Allfilms were soluble with an insoluble border. In an embodiment, a filmwith an insoluble border can be made completely spreadable by punching ashape from the region contained within the soluble section.

Example 8. Caffeine Films with Vitamin C of the Present Disclosure

FIGS. 91A-91B are fables summarizing embodiments of caffeine films ofthe present disclosure. Films were cast with 0.5%, 1%, 2.5%, 5%, 10%,15% and 20% caffeine and 20% or 25% vitamin C. All combinations formedfilms. 20% caffeine films had caffeine precipitate out. Films with0.5%-2.5% were soluble. In an embodiment, a caffeine film of the presentdisclosure is used for reducing puffy eyes.

Example 9. Caffeine Gels with Vitamin C of the Present Disclosure

A silk gel with 2% silk and 100 mg L-ascorbic acid/15 mL solution wascreated with the addition of 50 mg caffeine/15 mL solution. The gel hasthe exact appearance of standard L-ascorbic acid gels. In an embodiment,a caffeine gel of the present disclosure is used for reducing puffyeyes. A range of essential oils can be used including, but not limitedto, lemongrass, vanilla, geranium, and green tea.

Example 10. Green Tea Gels with Vitamin C of the Present Disclosure

Steps Green Tea Prep Heat 250 mL water to boil. Steep tea bag 2-3minutes with occasional stir. Remove tea bag and let cool. Gel SolutionPrep Use TFF-10-0047 (3.71% silk) dilute to 3% silk with water; diluteto 2% with green tea; add L- ascorbic acid. Gel Gelation occurred likestandard gel at room temperature. Green/yellow color. Green Tea scent.Solution Spec. 2% silk solution. 65 mL (35 ml of 3.71% silk, 8.3 mLwater, 21.66 mL green tea); 0.43 g L- ascorbic acid

FIG. 92 is a table summarizing an embodiment of a caffeine gel of thepresent disclosure. A silk gel with 2% silk and 100 mg L-ascorbicacid/15 mL solution was created with the addition of 50 mg caffeine/15mL solution. The gel has the exact appearance of standard L-ascorbicacid gels.

Example 11. Preservative Gels with Vitamin C of the Present Disclosure

FIG. 93 is a table summarizing embodiments of preservative gels of thepresent disclosure. Silk gels were cast with standard 2% silk solutionand 100 mg L-ascorbic acid/15 mL solution with the addition of apreservative and chelating agent. The preservative added was VerstatilSL by Kinetic (Water, Sodium Levulinate, Potassium Sorbate) at 1.5% andthe chelating agent was Dermofeel-PA3 by Kinetic (Sodium Phytate) at0.1%. The addition of preservatives extended gelation time to 7 days.Gel is being observed for discoloration and integrity with L-ascorbicacid and ascorbic acid-2-glucoside gel comparisons.

Example 12. Chemical Peels of the Present Disclosure

The primary variable investigated was the concentration of lactic acidand/or glycolic acid necessary to create a silk solution of a desiredpH. In order to determine the relationship between concentration in silkand pH, 2% silk solutions (60 minute boil, 25 kDA) were titrated withglycolic and lactic acid and tested for pH with pH strips. See thefollowing titrations/formulations below:

TABLE 26 Lactic Acid Peel 1: Initial solution: 25 mL of 2% silksolution, pH = 7-8 Quanity of Lactic Acid Added Total Lactic Acid pH 100μL 100 μL 3 100 μL 200 μL 2 100 μL 300 μL 1-2 Time to gel: 3 days

TABLE 27 Lactic Acid Peel 2: Initial solution: 25 mL of 2% silksolution, pH = 7-8 Quanity of Lactic Acid Added Total Lactic Acid pH 25μL 25 μL 4 Time to gel: >5 days

TABLE 28 Glycolic Acid Peel 1: Initial solution: 25 mL of 2% silksolution, pH = 7-8 Quanity of Glycolic Acid Added Total Glycolic Acid pH41 mg 41 mg 4 43.25 mg 84.25 mg 3 30.7 mg 114.95 mg 3 56.4 mg 171.35 mg2-3 91.66 mg 263.01 mg 2 171.35 mg 434.4 mg 1-2 Time to gel: 3 days

TABLE 29 Glycolic Acid Peel 2: Initial solution: 25 mL of 2% silksolution, pH = 7-8 Quantity of Lactic Acid Added Total Lactic Acid pH 41mg 41 mg 4 Time to gel: >5 days

TABLE 30 Lactic/Glycolic Acid Peel: Initial solution: 25 mL of 2% silksolution, pH = 7-8 Total Lactic Acid Total Glycolic Acid Lemongrass pH150 μL 200 mg 33.3 μL 2 Time to gel: 3 days

TABLE 31 Lactic/Glycolic Acid Peel: Initial solution: 30 mL of 2% silksolution, pH = 7-8 % Silk Solution (60 minute boil, 25 kDA) 2% LacticAcid Concentration 6 μL/mL Glycolic Acid Concentration 8 mg/mL pH 2Lemongrass Concentration 1.33 μL/mL

A peel of the present disclosure can have a % silk ranging from about0.5% to about 8%. The pH of a peel of the present disclosure can beadjusted with varying quantities of lactic and glycolic acid. Peels canalso be made with lactic acid only or glycolic acid only, A peel of thepresent disclosure can be clear/white in color. A peel of the presentdisclosure can have a gel consistency that is easily spread and absorbedby the skin. A peel of the present disclosure does not brown or changecolors.

In an embodiment, a chemical peel of the present disclosure can beapplied weekly to reveal healthy, vibrant skin. In an embodiment, achemical peel of the present disclosure can be applied weekly todiminish fine lines. In an embodiment, a chemical peel of the presentdisclosure can be applied weekly to firm the skin.

Each formulation (after titration, if applicable) was applied as aliquid and as a gel and observed for look and feel. Peels of pH=4(Lactic Acid Peel 2, Glycolic Acid peel 2) resulted in a minimal burningfeeling after a few minutes of application, while peels of pH=˜2 (LacticAcid Peel 1, Glycolic Acid Peel 1, Lactic/Glycolic Acid Peel) caused aslightly more intense burning feel. Little difference in degree ofburning was felt between liquid and gel other than that the burningsensation was more delayed in the gel form. PH was maintained in the gelform and was confirmed by using a pH strip.

Glycolic acid and lactic acid are both alpha hydroxy acids (AHAs) thatare among the most commonly used peels for superficial peeling(outermost skin layer peeling). Chemical peels are intended to burn thetop layers of the skin in a controlled manner, to remove superficialdermal layers and dead skin in order to improve appearance. AHAs arecommon in chemical peels due to low risk of adverse reactions and highcontrol of strength (control pH and time applied). Glycolic acid is mostcommonly used and has a very small molecular size, enabling deeppenetration into the epidermis. Lactic acid is another commonly used AHAand offers a more gentle peel with higher control due to its largermolecular size. Any number of chemicals known in the art that lower pHand are physical exfoliates can be used in place of AHAs.

Example 13. Hydrating Serums of the Present Disclosure

Variables include: concentration of silk in solution, concentration ofHA, addition

15 of vitamin C, and serum preparation method. Table 32 is a list ofsamples that were evaluated:

TABLE 32 Embodiments of serums of the present disclosure containing HAand Silk (60 minute boil, 25 kDA), with or without vitamin C, and with20 μL/15 mL lemongrass essential oil (30 mL solution) Method HA (%) Silk(%) Vit C (mg) Observation HA added to 0.5 2 0 White, slightly opaque,viscous liquid water before 1 White/yellow, slightly opaque, viscousdilution of silk liquid 0.5 2 0 Low viscosity, clear-white opaque withfilm on top, some white residue when applied topically to skin 1Slightly viscous, clear liquid with film on top 0.5 1 0 Slightlyviscous, clear liquid with film on top 1 Smooth viscous liquid, no whiteresidue when applied topically to skin 0.5 0.5 0 Moderately viscousliquid, clear 1 Smooth, clear, no white residue when applied topicallyto skin 0.5 2 35 Non homogeneous mix of hard gel and viscous liquid 1Non homogeneous mix of hard gel and viscous liquid 1 1 35 Nonhomogeneous mix of hard gel and viscous liquid 0.5 Opaque, whiteliquid/non-viscous 1 4 35 Separated mixture of hard gel and viscousliquid 0 Non homogeneous mix of hard gel and viscous liquid 5 2 0Yellow, gel HA added to 10 2 0 Viscous jelly upon stirring with waterbefore undissolved HA dilution of 5 Very viscous jelly upon stirringsilk, stirred 1 Viscous jelly upon stirring vigorously 0.5 HA added to 12 0 Non homogeneous thick, viscous jelly/gel water before 5 1 0 dilutionof silk, shaken HA added to 1 1 0 Clear/slightly opaque, viscous liquid,water and let smooth feel, little to no white residue sit for 1 day whenapplied topically to skin before dilution of silk HA added to 0.5 2 0Viscous, clear/white liquid varying in diluted silk 1 consistencysolution, 0.5 1 Clear viscous liquid varying in stirred 1 consistency0.5 6 White, opaque jelly varying in 1 consistency HA added to 0.5 3.9 0White, slightly opaque, viscous liquid diluted silk 1 solution, 0.5 2 35White gel varying in consistency stirred 1

In an embodiment, a hydrating serum of the present disclosure protectsthe skin and seals in moisture with the power of silk fibroin-basedfragment proteins. In an embodiment, a hydrating serum of the presentdisclosure delivers moisture for immediate and long-term hydrationthroughout the day with concentrated hyaluronic acid. A range ofessential oils can be used in a hydrating serum of the presentdisclosure including, but not limited to, lemongrass, vanilla, geranium,and green tea. In an embodiment, one or two drops of a hydrating serumof the present disclosure can be smoothed over the face and neck. In anembodiment, a hydrating serum of the present disclosure includes water,aqueous silk fibroin-based fragment solution, hyaluronic acid, andlemongrass oil. In an embodiment, the silk fibroin-based fragmentprotein in a hydrating serum of the present disclosure has the abilityto stabilize and protect skin while sealing in moisture, ail without theuse of harsh chemical preservatives or synthetic additives. In anembodiment, the hyaluronic acid in a hydrating serum of the presentdisclosure nourishes skin and delivers moisture for lasting hydration.In an embodiment, the lemongrass essential oil in a hydrating serum ofthe present disclosure yields antioxidant and anti-inflammatoryproperties that support skin rejuvenation. In an embodiment, a hydratingserum of the present disclosure has a pH of about 6.0.

Silk Fibroin-Based Fragment Solution

Because silk fibroin-based fragment solution is both aqueous and able toentrap and deliver small molecules, the solution is able to deliver bothwater and hygroscopic HA molecules to the skin for hydration. A range inconcentration of silk fibroin-based fragment compositions in solutionfrom 0.5%-6.0% was tested for feasibility and product outcome. Allconcentrations tested were found to be feasible.

Hyaluronic Acid

Hyaluronic acid (Sodium Hyaluronate) was tested as an ingredient in thehydrating serum due to its hygroscopic properties and ability to promotesoft, hydrated skin. A range in concentration of hyaluronic acid insolution from 0.5%-10.0% was tested for feasibility and product outcome.All concentrations tested, with the exception of 10.0%), were found tobe feasible. Feasibility was determined based on the ability to dissolvehyaluronic acid.

Vitamin E and Derivatives Thereof

Vitamin C (L-ascorbic acid) was tested as an ingredient in the hydratingserum. Initial vitamin C samples became a non-homogeneous mixture of geland liquid. A follow-up trial with vitamin C resulted in a homogeneous,white, opaque, non-viscous liquid that was not quickly absorbed by theskin, in an embodiment, a vitamin C derivative that does not readilycause gelation, such as sodium ascorbyl phosphate, could be added up tothe concentration at which it would no longer be soluble (for example,0% to about 40%). In an embodiment, 20% sodium ascorbyl phosphate couldbe added. Vitamin C options that do cause gelation (L-ascorbic acid andascorbyl glucoside) could be added at high concentrations (for examplegreater than about 10% up to about 50%) at which gelation is inhibited.

Serum Creation Method

Initial serums were created by the addition of HA to a silkfibroin-based fragment solution followed by stirring. The HA appeared tostick together and was not dissolved until forcefully stirred. Themixing process was then changed so that HA was first dissolved in waterand then immediately used to dilute a high concentration silkfibroin-based fragment solution (>4%) to the desired concentrations. Theresulting serums were more homogeneous and had a desirable smooth, clearlook and feel. Upon application to the skin, a white residue brieflyappeared that could be rubbed in. In an alternate method formulationswere created by dissolving HA in water and allowing it to sit for 1 dayuntil complete dissolution was observed. The HA and water solution wasthen used to dilute a high concentration silk fibroin-based fragmentsolution to the desired concentrations. The resulting serum was clear,smooth, homogeneous and left little to no white residue when applied.

Example 14. UV Hydrating Serums of the Present Disclosure

Variables tested include: concentration of HA, concentration of zincoxide, concentration of titanium dioxide, addition of vitamin C, andserum preparation method.

FIGS. 94A-94C are tables summarizing embodiments of cosmetic serums ofthe present disclosure with varying additives and concentrations ofcomponents suitable for protection against ultraviolet radiation (UV).Table 33 provides an embodiment of a hydrating serum of the presentdisclosure with vitamin C.

TABLE 33 Embodiment of Hydrating serum of the present disclosure withvitamin C % Silk Solution (60 minute boil, 25 kDA) 1.0% w/v HyaluronicAcid (sodium hyaluronate) 0.75% w/v Lemongrass Oil 20 uL/15 mL silksolution Sodium Ascorbyl Phosphate 6 g Lactic Acid 1.2 mL

A serum of the present disclosure can be made with from about 0.25% toabout 10% sodium hyaluronate (increasing % results in more viscousserum). 0.5% to about

10% silk solutions can be used to prepare a serum of the presentdisclosure. A serum of the present disclosure can be clear and have ayellow tinted color, A. serum of the present disclosure can have a pH=6.A serum of the present disclosure can have a lubricious texture that isrubbed in easily without residue,

Concentration of HA

Hyaluronic acid (Sodium Hyaluronate) was tested as an ingredient in theUV silk serum due to its hygroscopic properties and widely accepted usein cosmetic products to promote hydration of skin. 1%, 2.5% and 5% HAsolutions were tested. With increasing HA %, the serum became moreviscous and gel like. 1% HA was not feasible for the UV serum due to thefact that the UV additives (zinc oxide, titanium dioxide) are not watersoluble and need to be dispersed. 1% HA was not viscous enough fordispersion and the UV additives precipitated out, 2.5% gave the bestconsistency based on preferred feel, texture and viscosity and was ableto disperse the UV additives, 5% was a very thick, viscous serum.

Concentration of Mineral Filters: Zinc Oxide and Titanium Dioxide:

Zinc oxide and titanium dioxide were explored as UV additives that areconsidered safe. These additives mechanically protect from U radiationby forming a physical reflective barrier on the skin. Both are notsoluble in water and must be dispersed for the current aqueous solution.Zinc oxide concentration varied from 2.5%, 3.75%, 5%), 5.625%), 10%, 12%and 15%. Titanium dioxide concentrations varied from 1.25%, 1.875%), 3%,5% and 10%), increasing the concentration of UV additives resulted inminor increases of white residue and how well dispersed the additiveswere, however if mixed well enough the effects were negligible. Zincoxide and titanium dioxide were mixed together into serums in order toachieve broad spectrum protection. Zinc oxide is a broad spectrum UVadditive capable of protecting against long and short. UV A and UV Brays. However titanium dioxide is better at UV B protection and oftenadded with zinc oxides for best broad spectrum protection. Combinationsincluded 3.75%/1.25% ZnO/TiO₂, 5.625%/1.875% ZnO/TiO₂, 12%/3% ZnO/TiO₂,15%/5% ZnO/TiO₂. The 3.75%/1.25% ZnO/TiO₂ resulted in spf 5 and the5.625%/1.875% ZnO/TiO₂ produced spf 8.

Vitamin C:

Sodium ascorbyl phosphate was used as a vitamin C source. Formulationswere created with the vitamin C concentration equal to that in the silkgel (0.67%). Formulations were also created with 20% sodium ascorbylphosphate which is soluble in water.

Serum Preparation:

The vitamin C (sodium ascorbyl phosphate) must first be dissolved inwater. Sodium hyaluronate is then added to the water, mixed vigorouslyand left to fully dissolve. The result is a viscous liquid (depending onHA %). The viscosity of the HA solution al lows even dispersion of thezinc oxide and titanium dioxide and therefore HA must be mixed beforeaddition of UV additives. The zinc oxide and titanium dioxide are thenadded to the solution and mixed vigorously with the use of an electricblender. Silk solution is then added and mixed to complete the serumformulation.

Chemical Filters:

A UV serum of the present disclosure can include one, or a combinationof two or more, of these active chemical filter ingredients: oxybenzone,avobenzone, octisalate, octocrylene, homosalate and octinoxate. A UVserum of the present disclosure can also include a combination of zincoxide with chemical filters.

In an embodiment, a UV serum of the present disclosure can be appliedapproximately 15 minutes before sun exposure to all skin exposed to sun,and can be reapplied at least every 2 hours. In an embodiment, a UVserum of the present disclosure includes water, zinc oxide, sodiumhyaluronate, titanium dioxide, silk, and vitamin C or a vitamin Cderivative such as sodium ascorbyl phosphate, in an embodiment, a UVserum of the present disclosure protects skin and seals in moisture withthe power of silk protein. In an embodiment, a UV serum of the presentdisclosure improves skin tone, promotes collagen production anddiminishes the appearance of wrinkles and fine lines with theantioxidant abilities of vitamin C. In an embodiment, a UV serum of thepresent disclosure delivers moisture for immediate and long-termhydration throughout the day with concentrated hyaluronic acid. In anembodiment, a UV serum of the present disclosure helps prevent sunburnwith the combined action of zinc oxide and titanium dioxide. In anembodiment, a UV serum of the present disclosure is designed to protect,hydrate, and diminish fine lines while shielding skin from harsh UVA andUVB rays. In an embodiment, the silk protein in a UV serum of thepresent disclosure stabilizes and protects skin while sealing inmoisture, without the use of harsh chemical preservatives or syntheticadditives. In an embodiment, the vitamin C/derivative in a UV serum ofthe present disclosure acts as a powerful antioxidant that supports skinrejuvenation. In an embodiment, the sodium hyaluronate in a UV serum ofthe present disclosure nourishes the skin and delivers moisture forlong-lasting hydration. In an embodiment, the zinc oxide and titaniumdioxide in a UV serum of the present disclosure shields skin fromharmful UVA and UVB rays. The silk protein stabilization matrix in a UVserum of the present disclosure protects the active ingredients from theair, to deliver their foil benefits without the use of harsh chemicalsor preservatives. The silk matrix also traps moisture within the skinfurthering the hydrating effect of the sodium hyaluronate.

Example 15. Dark Spot Films of the Present Disclosure

To reduce the appearance of dark spots, a high concentration of vitaminC may be necessary to reverse the overproduction of melanin. In thisexample, a 40% vitamin C (1.5:1 silk to vitamin C) was studied. The sizeand shape of the film can be made appropriate to a targeted area, forexample to a small circular film of diameter 1 in (2.54 cm).

The dark spot film, or a similar film of the present disclosure, ofvarying vitamin C concentration (0-50%) can be applied as a hydrofilm.Skin can be wetted with water. The film is then applied to the wet area.Water is then applied to the top surface of the film to turn it into agel. The gel can then be spread and gently massaged into the applicationarea. Table 34 provides details of an embodiment of a hydrofilm of thepresent disclosure (with no insoluble border).

TABLE 34 An Embodiment of a hydrofilm of the present disclosure % SilkSolution (60 minute boil, 25 kDA) 2.56% Quanity Vitamin C (l-ascorbicacid) 15.62 mg total (10 mg in 1 in circle punch out) Volume of solutionper mold 2.44 mL Film Size 1.25 in diameter circle (7.917 cm{circumflexover ( )}2)

A film of the present disclosure can be made with different combinationsof % silk and volume to produce films with silk quantities of 3 mg/cm²to 10 mg/cm². A film of the present disclosure can be made with fromabout 1% to about 50% 1-ascorbic acid. A film of the present disclosureis soluble in water (insoluble border is removed by punching out thecenter of the film). A film of the present disclosure can adhere to skinwith water. A film of the present disclosure can be spread on skin oncewater is applied. A. film of the present disclosure can be dried whenthe humidity of drying equipment is 16-40%) and below the humidity ofthe lab. A film of the present disclosure can be clear/transparent.

In an embodiment, a dark spot film of the present disclosure includeswater, silk, and vitamin C (L-ascorbic acid). In an embodiment, a darkspot film of the present disclosure includes 40% vitamin C, In anembodiment, a dark spot film of the present disclosure reduces skinpigmentation and evens skin tone in a targeted area with daily-use.Vitamin C can inhibit pigment transfer from pigment producing cells,called melanocytes, to skin surface cells with continual application. Inan embodiment, a dark spot film of the present disclosure can be appliedto clean, dampened skin for 20 minutes. In an embodiment, additionalwater can be applied to an adhered film. The silk protein stabilizationmatrix in a dark spot film of the present disclosure protects the activeingredients from the air, to deliver their full benefits without the useof harsh chemicals or preservatives, such as paraben and phthalate.Thus, a dark spot film of the present disclosure is paraben andphthalate-free. Table 35 provides details of an embodiment of a film ofthe present disclosure.

TABLE 35 An Embodiment of a Film of the Present Disclosure % SilkSolution (60 minute boil, 25 kDA) 2.2% Surface area 5.07 cm{circumflexover ( )}2 Volume of silk solution for casting 1.56 mL Mass of silk perfilm: 34 mg Mass of l-ascorbic acid per film: 23 mg Concentration ofl-ascorbic acid in film:  40% pH 3

A 2.1% silk solution of the present disclosure (0.321 mL/cm²) to 2.4%silk solution of the present disclosure (0.282 mL/cm²) can been used tocreate dark spot films of the present disclosure with 34 mg of silk (6.7mg cm²). in an embodiment, a 2.2% silk solution of the presentdisclosure (60 minute boil, 25 kDA) is used to produce a film of thepresent disclosure. The % silk and volume of solution can vary toproduce equivalent films. A dark spot film of the present disclosure canbe made with different combinations of % silk and volume to producefilms with silk quantities of 3 mg/cm² to 10 mg/cm². A dark spot film ofthe present disclosure can be made with from about 15 to about 50%1-ascorbic acid. A dark spot film of the present disclosure is solublein water (insoluble border). A dark spot film of the present disclosureis clear/transparent. A dark spot film of the present disclosure has a

when water is applied. A dark spot film of the present disclosure canadhere to skin with water. A dark spot film of the present disclosurecan dry when humidity of drying equipment is 16-40% and below thehumidity of the lab

Example 16. High Concentration Vitamin C Gels of the Present Disclosure

High concentration vitamin C gels were pursued up to 20%). Vitamin Ctype, vitamin C concentration, % silk and pH were varied to increase thequantity of vitamin C in a gel.

FIGS. 95A-95C are tables summarizing embodiments of high concentrationvitamin C gels of the present disclosure. The highest concentration ofvitamin C to gel was a 15% ascorbic acid 2 glucoside gel with 3.8% silksolution after 12 days. 5 and 10% ascorbic acid-2-glucoside formulationswith 2, 3 and 3.8% silk all gelled. For each group of % vitamin C,gelation first occurred in the 3.8% silk followed by the 3%) and lastlythe 2%. It appears that there is a relationship between vitamin Cconcentration, silk concentration and gelation. If a solution has toomuch vitamin C in relation to silk, gelation will be prevented.Therefore, in order to produce high concentration vitamin C gels, higherconcentration silk is necessary. One sample was cast at 5.5% silk and20% vitamin C but gelation did not occur and a higher % silk may benecessary. Samples were also brought to a pH of 2 with lactic acid inorder to help induce gelation in 3% silk solutions with 10 or 20%vitamin C, however gelation did not occur in 12 days.

Example 17. Microbiological Study of Gels of the Present Disclosure

Contaminating micro-organisms in cosmetics may cause a spoilage of theproduct and, when pathogenic, they represent a serious health risk forconsumers worldwide. The United States Pharmacopoeia (USP) MicrobialLimits Test provides several methods for the determination of totalmicrobial count for bacteria, yeast and mold. Various gels of thepresent disclosure were tested to evaluate the possible microbialcontamination in three different states of their use (intact, in-use,ending product). FIG. 96 is a table summarizing the results of suchtesting.

The samples of gel and water samples from carboys were analyzed fordetermination of CFU/mL (colony-forming units per milliliter) of aerobicbacteria as well as yeast and mold. Samples were exposed to growthmedium of Tryptic Soy Agar (TSA) for bacteria and Potato Dextrose Agar(PDA) for fungi (yeast/mold) at an exposure temperature of 23±3° C.Samples were incubated at 30.0±2° C. for 3 days (bacteria) and 5 days(Fungi). Samples were then observed for determination of colony-formingunits/mL.

The limit of detection for the assays was 10 CFU/ml or g for bacteriaand fungi, and the values of <10 indicate that microorganisms could notbe detected in the samples. Values of >1.00E+04 indicate that themicrobial colonies are Too Numerous to Count in the dilutions plated.

Example 18. UV Silk Foams and Liquids of the Present Disclosure

In an embodiment, the vitamin C derivative sodium ascorbyl phosphate(DSM) was dissolved in water. Sodium hyaluronate (“HA”) was then addedto the water, mixed vigorously, and left to fully dissolve. The resultis a viscous liquid (depending on HA %), The viscosity of the HAsolution allows even dispersion of the zinc oxide and titanium dioxideand therefore HA is typically mixed before addition of UV additives. Thezinc oxide and titanium dioxide are added to the HA solution and mixedvigorously, for example with the use of an electric blender. 60 minuteboiled (−25 kDa) silk solution is then added and mixed to create a 1%silk formulation.

Two formulations were created without the addition of sodium ascorbylphosphate (samples “HU2” and “HU4”). For sample HU2, zinc oxide andtitanium dioxide were added and mixed by blending with an electricblender and whisk. The result was a viscous white liquid (FIG. 98 andFIG. 99). Silk was then added and blended with an electric blender andwhisk. The solution became a creamy foam similar to shaving cream (FIG.97 and FIG. 100). Vitamin E in the form of dl-alpha tocopheryl acetatecan be added to the solution to recover a viscous liquid texture thatcan be applied with a smooth even texture (FIG. 98). With increasing thequantity of dl-alpha tocopheryl acetate, the formulation will becomeless foam-like and more of a smooth liquid or lotion texture.

HU4 was split into two batches: FIG. 99, batch 2 and FIG. 100, batch 1.The first batch followed the same procedures to HU2 and became a foam.For the second batch of U4, sodium ascorbyl phosphate was added anddissolved before adding any zinc, titanium or silk. The UV additiveswere then added by blending with an electric blender and whisk andcreated a standard white viscous liquid. Silk was then added with, anelectric blender and whisk. The result was slightly thicker viscousliquid than normally seen. Without wishing to be bound by theory, itappears the addition of sodium ascorbyl phosphate inhibits foaming.Without wishing to be bound by theory, it appears that whisking, asopposed to mixing or blending, creates a silk foam.

TABLE 36 Embodiments of UV Silk Foams and Liquids of the PresentDisclosure % Sodium HA Mass Mass Mass Ascorbyl Total % (sodium HA % ZnO% TiO₂ Phosphate Sample Volume silk hyahironate) (g) ZnO (g) TiO₂ (g)(g) HU2 55 1 2.5 1.375 12 6.6 3 1.65 N/A HU4 27.5 1 3.5 0.9625 12 3.3 30.825 5.5 Batch 1 HU4 27.5 1 3.5 0.9625 12 3.3 3 0.825 N/A Batch 2

Example 19. Lyophilized Silk Powders of the Present Disclosure

TABLE 37 Embodiments of lyophilized silk powders Silk Solution TreatmentSoluble ~60 kDa silk, 6% silk, pH = 7-8 lyopholize and cut with noblender ~60 kDa silk, 6% silk, pH = 10 lyopholize and cut with noblender ~25 kDa silk, 6% silk, pH = 7-8 lyopholize and cut with yesblender ~25 kDa silk, 6% silk, pH = 10 lyopholize and cut with yesblender

The above silk solutions were transformed to a silk powder throughlyophilization to remove bulk water and chopping to small pieces with ablender. pH was adjusted with sodium hydroxide. Low molecular weightsilk (−25 kDa) was soluble while high molecular weight silk (−60 kDa)was not.

The lyophilized silk powder can be advantageous for enhanced storagecontrol ranging from 10 days to 10 years depending on storage andshipment conditions. The lyophilized silk powder can also be used as araw ingredient in the pharmaceutical, medical, consumer, and electronicmarkets. Additionally, lyophilized silk powder can be re-suspended inwater, HFIP, or an organic solution following storage to create silksolutions of varying concentrations, including higher concentrationsolutions than those produced initially.

In an embodiment, aqueous pure silk fibroin-based protein fragmentsolutions of the present disclosure comprising 1%, 3%, and 5% silk byweight were each dispensed into a 1.8 L Lyoguard trays, respectively.All 3 trays were placed in a 12 ft² lyophilizer and a single runperformed. The product was frozen with a shelf temperature of ≤−40° C.and held for 2 hours. The compositions were then lyophilized at a shelftemperature of −20° C., with a 3 hour ramp and held for 20 hours, andsubsequently dried at a temperature of 30° C., with a 5 hour ramp andheld for about 34 hours. Trays were removed and stored at ambientconditions until further processing. Each of the resultant lyophilizedsilk fragment compositions were able to dissolve in aqueous solvent andorganic solvent to reconstitute silk fragment solutions between 0.1 wt %and 8 wt %. Heating and mixing were not required but were used toaccelerate the dissolving rate. All solutions were shelf-stable atambient conditions.

In an embodiment, an aqueous pure silk fibroin-based protein fragmentsolution of the present disclosure, fabricated using a method of thepresent disclosure with a 30 minute boil, has a molecular weight ofabout 57 kDa, a polydispersity of about 1.6, inorganic and organicresiduals of less than 500 ppm, and a light amber color.

In an embodiment, an aqueous pure silk fibroin-based protein fragmentsolution of the present disclosure, fabricated using a method of thepresent disclosure with a 60 minute boil, has a molecular weight ofabout 25 kDa, a polydispersity of about 2.4, inorganic and organicresiduals of less than 500 ppm, and a light amber color.

Example 20. Formulation of Moisturizing Composition

In an embodiment, a moisturizing composition comprises:

Water 65%-99% w/v 6% Silk solution 0.1%-5% v/v Hyaluronic acid 0.1%-5%w/v Jojoba Oil 0%-25% v/v Rosehip Oil 0%-25% v/v Vitamin E 0%-5% v/vAspen bark 0.5%-2% w/v Sodium Anisate 0.1%-1% w/v 5N NaOH 0.1%-0.5% 2MHCl 0.5%-1.5% Glycerin 0%-10% v/v Coconut Oil 0%-25% v/v Lemongrass Oil0%-25% v/v Shea butter 0%-25% v/v Oat flour 0%-5% w/v Titanium Oxide0%-5% w/v Zinc Oxide 0%-5% w/v

Example 21. Formulation of Moisturizing Composition

In an embodiment, a moisturizing composition comprises:

Water 65%-99% w/v 6% Silk solution 0.1%-5% v/v Hyaluronic acid 0.1%-5%w/v Jojoba Oil 0%-25% v/v Rosehip Oil 0%-25% v/v Vitamin E 0%-5% v/vAspen bark 0%-5% w/v Sodium Anisate 0.1%-1% w/v 5N NaOH 0.1%-0.5% 2M HCl0.5%-1.5%

Example 22. Formulation of Moisturizing Composition

In an embodiment, a moisturizing composition comprises:

Water 65%-99% w/v 6% Silk solution 0.1%-5% v/v Hyaluronic acid 0.1%-5%w/v Jojoba Oil 5%-15% v/v Rosehip Oil 5%-15% v/v Vitamin E 0.5%-2% v/vAspen bark 0.5%-2% w/v Sodium Anisate 0.1%-1% w/v 5N NaOH 0.1%-0.5% 2MHCl 0.5%-1.5%

Example 23. Formulation of Moisturizing Composition

In an embodiment, a moisturizing composition comprises:

Water 65%-99% w/v 6% Silk solution 0.1%-5% v/v Hyaluronic acid 0.1%-5%w/v Oil or butter 0.1%-25% v/v pH adjusting agent 0.1%-1.5% v/v

Example 24. Formulation of Moisturizing Composition

In an embodiment, a moisturizing composition comprises:

Water 65%-99% w/v Silk protein fragments 0.01%-1% w/v Hyaluronic acid0.1%-5% w/v Jojoba Oil 5%-15% v/v Rosehip Oil 5%-15% v/v Vitamin E0.5%-2% v/v 5N NaOH 0.1%-0.5% 2M HCl 0.5%-1.5%

Example 25. Formulation of Moisturizing Composition

In an embodiment, a moisturizing composition comprises:

Water 65%-99% w/v Silk protein fragments 0.01%-1% w/v Hyaluronic acid0.1%-5% w/v Jojoba Oil 0%-25% v/v Rosehip Oil 0%-25% v/v Vitamin E 0%-5%v/v Aspen bark 0%-5% w/v Sodium Anisate 0.1%-1% w/v 5N NaOH 0.1%-0.5% 2MHCl 0.5%-1.5%

Example 26. Formulation of Moisturizing Composition

In an embodiment, a moisturizing composition comprises:

Water 65%-99% w/v Silk protein fragments 0.06%-0.2% w/v Hyaluronic acid0.1%-5% w/v Jojoba Oil 0%-25% v/v Rosehip Oil 0%-25% v/v Vitamin E 0%-5%v/v Aspen bark 0%-5% w/v Sodium Anisate 0.1%-1% w/v 5N NaOH 0.1%-0.5% 2MHCl 0.5%-1.5%

Example 27. Moisturizer Composition User Testing

A trial was conducted with 9 people on a moisturizer composition of thepresent disclosure. Six respondents (67% of respondents) reported usingthe moisturizer once a day. Three respondents reported using themoisturizer twice a day. No respondents reported using the moisturizermore than twice a day.

All respondents used the moisturizer in the morning and/or night. Therewas not a very strong preference between morning and night althoughmorning was most popular. Four respondents reported only applying themoisturizer in the morning. Two respondents reported only applying themoisturizer at night. Three respondents reported applying themoisturizer both in the morning and at night.

Three respondents reported applying a serum before applying themoisturizer; in one case a respondent reported using a “complex c serum”before applying the moisturizer. Five respondents reported that they didnot apply a serum before applying the moisturizer, while one respondentreported sometimes applying a serum before applying the moisturizer.Most respondents did not use a treatment serum before application of themoisturizer.

Four respondents reported applying makeup over the moisturizer. Threerespondents reported they did not apply makeup over the moisturizer. Tworespondents reported they sometimes applied makeup over the moisturizer.Most respondents did apply makeup over the moisturizer.

All respondents expressed that the moisturizer did moisturize the skin.33% of respondents commented on how the moisturizer did not feelgreasy/oily. 66% of respondents referred to the feeling assmooth/silky/soft. The overall feedback was excited and positive.

88% of respondents (eight out of nine) said the application of themoisturizer was easy. The only negative response had a problem with thejar and spatula and would prefer a pump. Some respondents commented onthe ease of spreading and absorbing into the skin.

The general feedback/comments were very positive with 66% of responseslacking any negative comment. Multiple respondents asked to put theproduct into production immediately so they could have it. Therespondents also commented on the clean, smooth feel and desirabletexture and appearance.

Example 28. Formulation of Moisturizing Composition

In an embodiment, a moisturizing composition that may provide a heavymoisturizer for intense hydration comprises:

Hyaluronic Acid 0.1-5% (w/v) 6% Silk Solution 0.1-25% (v/v) Water50%-99% (v/v) Shea Butter 0-40% (v/v) Coconut Oil 0-40% (v/v) Vitamin E0-5% (v/v) Aspen Bark 0-5% (w/v) Sodium Anisate 0.1-5% (w/v) 5N NaOH0.01-5% (v/v) 2M HCl 0.01-10% (v/v) ( )

Example 29. A Method for Manufacturing the Moisturizing Composition ofExample 28

The exemplary moisturizing composition provided in Example 28 may beprovided according to the following process.

Prepare a Pre-Casting Solution:

Prepare the hyaluronic acid (HA) solution:

Pour 68.2% (±1.0%) v/v of RO/DI water into a clean beaker (e.g., 1000 mLof solution*0.682=682 mL RO/DI water).

Use a mixer to gently stir the RO/DI water (e.g., <600 rpm with anoverhead lab mixer for 2500 mL batch size). Slowly add 1.64% (±0.02%)w/v hyaluronic acid powder to the RO/DI water (e.g., 1000 mL ofsolution*0.0164=16.4 g hyaluronic acid powder).

Once all of the HA has been added, use a mixer to mix the RO/DI waterand HA vigorously until the HA is fully dissolved (e.g., 1000-2000 rpmwith an overhead lab mixer for 2500 mL batch size. Use a speed thatcreates mixing throughout the entire volume of solution withoutsplashing).

The HA powder may need to be scraped off of sides of container andstirrer after initial mixing with the use of a spatula. Undissolved HApowder will appear as white powder or concentrated groups of smallbubbles. The HA is fully dissolved when the mixture is completelyhomogenous and has a consistent fluid flow per visual assessment. Checkhomogeneity by rotating and/or rocking the mixing container. HA powderwill typically dissolve completely in 1-3 hours of vigorous mixing time.

Prepare the hyaluronic acid/silk solution:

To the RO/DI Water and HA mixture, add 4.3% (±0.01%) v/v 6.0% silk(e.g., 1000 mL of solution*0.043=43 mL 6.0% silk).

Use a mixer to gently mix the solution until it is completelyhomogeneous per visual assessment (e.g., 100-400 rpm for a 2500 ml batchsize with an overhead lab mixer). It typically takes approximately 5-10minutes to reach complete homogeneity.

Store the hyaluronic acid/silk solution in a refrigerator overnight (atleast 12 hours). Solution may be transferred to another container.

Prepare the Casting Solution:

Add the hyaluronic acid solution to a plastic or glass beaker if it isnot already in an appropriate beaker or bowl.

In two separate beakers heat 12.8% (±0.1%) w/v shea butter (e.g., 1000mL of solution*0.128=128 mL shea butter) and 12.8% (±0.1%) w/v coconutoil (e.g., 1000 mL of solution*0.128=128 mL coconut oil) in a 75° C.laboratory oven to dissolve (approximately 30 min to 1 hour).

While the shea butter and coconut oil are heating, heat the hyaluronicacid/silk solution to 50° C. (±5° C.) with the use of a hot plate or laboven. If using a hot plate, be sure to mix the solution gently with theuse of a lab mixer so that the heated solution is evenly dispersed.

In a separate beaker mix to combine the heated shea butter and coconutoil, 0.9% (±0.01%) v/v Vitamin E (e.g., 1000 mL of solution*0.009=9 mLVitamin E) and 0.206% (±0.001%) v/v 5N NaOH (e.g., 1000 mL ofsolution*0.00206=2.06 mL 5N NaOH). Mix for approximately 10 seconds(Note: may mix by hand).

Use a mixer to mix the hyaluronic acid/silk solution at a power of300-800 rpm (overhead lab mixer) while the beaker is being heated with ahot plate at a heat setting of 3-5.

Mixing power and hot plate setting will be determined by batch size. Amixing speed that creates gentle mixing and agitation should be used.

Add the shea butter, coconut oil, vitamin E and 5N NaOH mixture to themixing hyaluronic acid/silk solution. Increase mixing speed to createvigorous mixing and agitation (1200-2000 rpm for 2500 mL batch size).Mix until the solution is a white, lotion like, homogenous mixture.Continue to mix for at least 20 minutes.

Remove the solution from the hot plate and continue to stir. Immediatelyadd 0.72% (±0.001%) v/v 2M Hydrochloric Acid (HCl) (e.g., 1000 mL ofsolution*0.0072=7.2 mL 2M HCl).

As the 2M HCl is added, the solution will become very sticky andviscous. Some solution may stick to the mixing attachment. Periodically,stop mixing and remove the solution that is stuck to the attachment withthe use of a spatula and continue mixing until mixture is homogenous.

Use a mixer to mix the solution vigorously (e.g. a power of 1000-2000rpm with an overhead lab mixer for 2500 mL batch size) for at least 30minutes.

Allow the solution to cool to less than 27° C. by leaving at roomtemperature or by placing in a refrigerator to speed cooling.

To the mixture, add 0.95% (±0.005%) w/v aspen bark (e.g., 1000 mL ofsolution*0.0095=95 g Aspen Bark). Use a mixer to mix vigorously untilthe aspen bark is completely dissolved per visual assessment (e.g.,speed of 6-10 for KitchenAid or 300-1500 rpm for an overhead lab mixer).Complete dissolution typically takes 10-20 minutes of vigorous mixingtime.

To the mixture, add 0.4% (±0.005%) w/v sodium anisate (e.g., 1000 mL ofsolution*0.004=4 g sodium anisate). Use a mixer to mix vigorously untilthe sodium anisate is completely dissolved per visual assessment (e.g.,speed of 6-10 for KitchenAid or 300-1500 rpm for an overhead lab mixer).Complete dissolution typically takes 10-20 minutes of vigorous mixingtime.

Casting Final Product:

Select and prepare clean product containers and arrange them for castingon a level surface. Dispense an appropriate volume of solution into acontainer.

Example 30. Formulation of Moisturizing Composition

In an embodiment, a moisturizing composition that may provide a lightermoisturizer for oily skin and a matte finish comprises:

Hyaluronic Acid 1.54% (w/v) (0.1-2.5%) 6% Silk Solution 1.75% (v/v)(0.1-25%) Water 86.8% (v/v) Rosehip Oil 5% (v/v) (0-15%) Jojoba Oil 5%(v/v) (0-15%) Vitamin E 0.9% (v/v) (0-5%) Aspen Bark 0.9% (w/v) (0.5%)Sodium Anisate 0.3% (w/v) (0.1-5%) 5N NaOH 0.15% (v/v) (0.01-5%) 2M HCl0.38% (v/v) (0.01-10%)

Example 31. A Method for Manufacturing the Moisturizing Composition ofExample 30

The exemplary moisturizing composition provided in Example 30 may beprovided according to the following process.

Prepare a Pre-Casting Solution:

Prepare the hyaluronic acid (HA) solution:

Pour 86.8% (±1.0%) v/v of RO/DI water into a clean beaker (e.g., 1000 mLof solution*0.868=868 mL RO/DI water).

Use a mixer to gently stir the RO/DI water (e.g., <600 rpm with anoverhead lab mixer for 2500 mL batch size). Slowly add 1.54% (±0.02%)w/v hyaluronic acid powder to the RO/DI water (e.g., 1000 mL ofsolution*0.0154=154 g hyaluronic acid powder).

Once all of the HA has been added, use a mixer to mix the RO/DI waterand HA vigorously until the HA is fully dissolved (e.g., 600-2000 rpmwith an overhead lab mixer for 2500 mL batch size. Use speed thatcreates mixing throughout the entire volume of solution withoutsplashing).

The HA powder may need to be scraped off of sides of container andstirrer after initial mixing with the use of a spatula. Undissolved HApowder will appear as white powder or concentrated groups of smallbubbles. The HA is fully dissolved when the mixture is completelyhomogenous and has a consistent fluid flow per visual assessment. Checkhomogeneity by rotating and/or rocking the mixing container. HA powderwill typically dissolve completely in 1-3 hours of vigorous mixing time.

Prepare the hyaluronic acid/silk solution:

To the RO/DI Water and HA mixture, add 1.75% (±0.01%) v/v 6.0% silk(e.g., 1000 mL of solution*0.0175=17.5 mL 6.0% silk).

Use a mixer to gently mix the solution until it is completelyhomogeneous per visual assessment (e.g., 100-400 rpm for a 2500 ml batchsize with an overhead lab mixer). It typically takes approximately 5-10minutes to reach complete homogeneity.

Store the hyaluronic acid/silk solution in a refrigerator overnight (atleast 12 hours). Solution may be transferred to another container.

Prepare the Casting Solution:

Add the hyaluronic acid solution to a plastic or glass beaker if it isnot already in an appropriate beaker.

In a separate beaker, mix to combine 5.0% (±0.1%) v/v jojoba oil (e.g.,1000 mL of solution*0.05=50 mL jojoba oil), 5.0% (±0.1%) v/v rosehip oil(e.g., 1000 mL of solution*0.05=50 mL rosehip oil), 0.9% (±0.01%) v/vVitamin E (e.g., 1000 mL of solution*0.009=9 mL Vitamin E) and 0.154%(±0.001%) v/v 5N NaOH (e.g., 1000 mL of solution*0.00154=1.54 mL 5NNaOH). Mix for approximately 10 seconds.

Use a mixer to mix the hyaluronic acid solution at a power 300-800 rpm(overhead lab mixer). Mixing power will be determined by batch size. Amixing speed that creates gentle mixing and agitation should be used.

Add the jojoba oil, rosehip oil, vitamin E and 5N NaOH mixture to thehyaluronic acid/silk solution. Increase mixing speed to create vigorousmixing and agitation (1200-2000 rpm for 2500 mL batch size). Mix untilthe solution is a white, lotion like, homogenous mixture. Continue tomix for at least 20 minutes.

To the mixture, add 0.38% (±0.001%) v/v 2M Hydrochloric Acid (HCl)(e.g., 1000 mL of solution*0.0038=3.8 mL 2M HCl).

As the 2M HCl is added, the solution will become very sticky andviscous. Some solution may stick to the mixing attachment. Periodically,stop mixing and remove the solution that is stuck to the attachment withthe use of a spatula and continue mixing until mixture is homogenous.

Use a mixer to mix the solution vigorously (e.g. a power of 1000-2000rpm with an overhead lab mixer for 2500 mL batch size) for at least 30minutes.

To the mixture, add 0.9% (0.005%) w/v aspen bark (e.g., 1000 mL ofsolution*0.009=9 g Aspen Bark). Use a mixer to mix vigorously until theaspen bark is completely dissolved per visual assessment (300-1500 rpmfor an overhead lab mixer (˜1000-1500 rpm for 2500 mL batch size)).Complete dissolution typically takes 10-20 minutes of vigorous mixingtime.

To the mixture, add 0.3% (0.005%) w/v sodium anisate (e.g., 1000 mL ofsolution*0.003=3 g sodium anisate). Use a mixer to mix vigorously untilthe sodium anisate is completely dissolved per visual assessment(300-1500 rpm for an overhead lab mixer (˜1000-1500 rpm for 2500 mLbatch size)). Complete dissolution typically takes 10-20 minutes ofvigorous mixing time

Casting Final Product:

Select and prepare clean product containers and arrange them for castingon a level surface. Dispense an appropriate volume of solution into eachcontainer.

Example 32. Formulation of Moisturizing Composition

In an embodiment, a moisturizing composition that may provide a bodymoisturizer comprises:

Hyaluronic Acid 1.75% (w/v) (0.1-5%) 6% Silk Solution 4.25% (v/v)(0.1-25%) Water 70% (v/v) Shea Butter 7.5% (v/v) (0-25%) Coconut Oil12.5% (v/v) (0-25%) Jojoba Oil 5% (v/v) (0-25%) Aspen Bark 0.95% (w/v)(0-5%) Sodium Anisate 0.4% (w/v) (0.1-5%) 5N NaOH 0.2% (v/v) (0.01-5%)2M HCl 0.7% (v/v) (0.01-10%)

Example 33. Formulation of Moisturizing Composition

In an embodiment, a moisturizing composition that may provide amoisturizer comprises:

Water 70-99% (w/v) 6% Silk Solution 0.1-5% (v/v) Jojoba Oil 0-25% (v/v)Rosehip Oil 0-25% (v/v) Vitamin E 0-5% (v/v) Aspen Bark 0.5-2% (w/v)Sodium Anisate 0.1-1% (w/v) 5N NaOH 0.1-0.5% (v/v) 2M HCl 0.5-1.5% (v/v)

Other ingredients for the moisturizing composition may include one ormore of:

Glycerin 0-10% (v/v) Coconut Oil 0-25% (v/v) Lemongrass Oil 0-25% (v/v)Shea Butter 0-25% (v/v) Oat Flour 0-5% (w/v) Titanium Oxide 0-5% (w/v)

Example 34: A Method for Manufacturing the Moisturizing Composition ofExample 33

In preparing a moisturizing composition of Example 33, an amount ofRO/DI water (X % v/v) may be added into a beaker or bowl (KitchenAid).An amount of hyaluronic acid powder (X % w/v) may be added to the RO/DIwater. The mixture may be vigorously mixed at a power of 6-10(KitchenAid) or 300-700 rpm (in a laboratory mixer) until the hyaluronicacid is fully dissolved (e.g., about 1 to 3 hours).

A 6% silk solution (X % v/v) may then be added to the preparedhyaluronic acid solution and mixed gently at a power of 2 (KitchenAid)or 50-80 rpm (in a laboratory mixer) until the silk and hyaluronic acidsolution are homogenous. The combined solution may then be stored in arefrigerator overnight. The solution can be transferred to anothercontainer.

The hyaluronic acid/silk solution may be added to a beaker or bowl(KitchenAid). To the prepared hyaluronic acid/silk solution may be addedjojoba oil (X % v/v), rosehip oil (X % v/v), Vitamin E (X % v/v), and 5NNaOH (X % v/v). The mixture may be stirred at a power of 4-10(KitchenAid) or 300-700 rpm (in a laboratory mixer). The mixture may bestirred until it provides a white, lotion like, homogenous mixture (seeFIGS. 101-107). The mixture may be stirred for about 10 minutes.

To the homogenous mixture may be added 2M HCl (X % v/v) and the mixturemay be stirred at a power of 4-10 (KitchenAid) or 300-700 rpm (in alaboratory mixer). The mixture may be stirred for at least 15 minutes.Aspen bark (X % w/v) may then be added to the mixture and stirred at apower of 4-10 (KitchenAid) or 300-700 rpm (in a laboratory mixer). Themixture may be stirred for at least 15 minutes. Sodium anisate (X % w/v)may then be added to the mixture and stirred at a power of 4-10(KitchenAid) or 300-700 rpm (in a laboratory mixer) for at least 15minutes to yield a product moisturizing composition.

Example 35: Moisturizer Shelf-Life Pilot Study

A shelf-life pilot study was performed to examine the shelf-lifestability of an exemplary moisturizing composition in both jars andpumps. Three 15 mL jars and three 30 mL pumps were filled with anexemplary moisturizing composition.

After one day, (1) the moisturizing composition in the jars was thick,opaque, uniform, and off-white in color (FIGS. 108); and (2) themoisturizing composition in the pumps was thick, opaque, uniform,off-white in color, and included air pockets.

After twenty days, (1) the moisturizing composition in the jars wasthick, opaque, uniform, and off-white in color (FIGS. 110); and (2) themoisturizing composition in the pumps was thick, opaque, uniform,off-white in color, and included air pockets (FIG. 111).

Accordingly, upon completion of the pilot study, the moisturizingcomposition in the jars and pumps exhibited no change in color,consistency, or uniformity from day one to day twenty.

Example 36. Formulation of Moisturizing Compositions

A series of 61 moisturizing compositions was prepared (FIG. 112) andexamined. Specifically, the moisturizing compositions were prepared withvarying amounts of silk (% silk (w/v)) in combination with a variety ofadditives (e.g., shea butter, jojoba, coconut oil, vitamin E, oatflour).

Example 37. Formulation of Sun Protectant

In an embodiment, a sun protection formulation that may provide a sunprotectant may be:

Water 74% (v/v) Hyaluronic Acid 1.74% (w/v) 6% Silk Solution 1.29% (v/v)Jojoba Oil 7.25% (v/v) Rosehip Oil 7.25% (v/v) Fractionated Coconut Oil1.80% (v/v) Coconut Oil 1.40% (v/v) Titanium Dioxide 4.50% (w/v) ZincOxide 4.50% (w/v) 5N NaOH 0.15% (v/v) 2M HCl 3.80% (v/v) pH Unknown

The resulting sun protection factor for the above-referenced formulationis 18.

Example 38. Formulation of a Sun Protectant

In an embodiment, a sun protection formulation that may provide a sunprotectant may be:

Water 74.60% (v/v) Hyaluronic Acid 1.70% (w/v) 6% Silk Solution 1.67%(v/v) Jojoba Oil 10.00% (v/v) Rosehip Oil 10.00% (v/v) Vitamin E 0.90%(v/v) Titanium Dioxide 5.00% (w/v) Zinc Oxide 5.00% (w/v) 5N NaOH 0.15%(v/v) 2M HCl 1.80% (v/v) Aspen Bark 0.90% (w/v) Sodium Anisate 0.40%(w/v) pH 7.11

The resulting sun protection factor for the above-referenced formulationis about 7.5 to 19.

Example 39. Formulation of a Sun Protectant

In an embodiment, a sun protection formulation that may provide a sunprotectant may be:

Water 12.10% (v/v) Hyaluronic Acid 1.00% (w/v) 6% Silk Solution 2.00%(v/v) Coconut Oil 20.00% (v/v) Shea Butter 35.00% (v/v) Raspberry SeedOil 5.00% (v/v) Vitamin E 0.90% (v/v) Glycerin 15.00% (v/v) TitaniumDioxide 3.50% (w/v) Zinc Oxide 3.50% (w/v) NaOH (pellets) 1.00% (w/v) 2MHCl 10.00% (v/v) pH 6.56

The resulting sun protection factor for the above-referenced formulationis about 20.

Example 40. Formulation of a Sun Protectant

In an embodiment, a sun protection formulation that may provide a sunprotectant may be:

Water 10.10% (v/v) Hyaluronic Acid 1.00% (w/v) 6% Silk Solution 2.00%(v/v) Coconut Oil 25.00% (v/v) Shea Butter 30.00% (v/v) Raspberry SeedOil 10.00% (v/v) Vitamin E 0.90% (v/v) Glycerin 10.00% (v/v) TitaniumDioxide 3.50% (w/v) Zinc Oxide 3.50% (w/v) NaOH (pellets) 75.00% (w/v)2M HCl 12.00% (v/v)

The resulting sun protection factor for the above-referenced formulationis about 18.

Example 41. Formulation of a Sun Protectant

In an embodiment, a sun protection formulation that may provide a sunprotectant may be:

Water 30.60% (v/v) 6% Silk Solution 1.50% (v/v) Jojoba Oil 25.00% (v/v)Coconut Oil 25.00% (v/v) Vitamin E 0.90% (v/v) Glycerin 15.00% (v/v)Titanium Dioxide 5.00% (w/v) Zinc Oxide 5.00% (w/v) 5N NaOH 1.80% (v/v)2M HCl 2.00% (v/v) Aspen Bark 0.90% (w/v) Sodium Anisate 0.40% (w/v)

Example 42. Formulation of a Sun Protectant

In an embodiment, a sun protection formulation that may provide a sunprotectant may be:

Water 14.10% (v/v) 6% Silk Solution 5.00% (v/v) Jojoba Oil 15.00% (v/v)Coconut Oil 25.00% (v/v) Shea Butter 25.00% (v/v) Vitamin E 0.90% (v/v)Glycerin 15.00% (v/v) Titanium Dioxide 4.00% (w/v) Zinc Oxide 4.00%(w/v) NaOH (pellets) 2.00% (w/v) 2M HCl 2.00% (v/v) Aspen Bark 0.90%(w/v) Sodium Anisate 0.40% (w/v) pH 7

Example 43. Formulation of a Sun Protectant

In an embodiment, a sun protection formulation that may provide a sunprotectant may be:

Water 10.10% (v/v) 6% Silk Solution 2.00% (v/v) Coconut Oil 29.00% (v/v)Shea Butter 35.00% (v/v) Vitamin E 0.90% (v/v) Glycerin 20.00% (v/v)Titanium Dioxide 4.00% (w/v) Zinc Oxide 4.00% (w/v) NaOH (pellets) 1.00%(w/v) 2M HCl 5.00% (v/v) Aspen Bark 0.90% (w/v) Sodium Anisate 0.40%(w/v) pH 7

Example 44. Formulation of a Sun Protectant

In an embodiment, a sun protection formulation that may provide a sunprotectant may be:

Water 10.10% (v/v) 6% Silk Solution 2.00% (v/v) Coconut Oil 10.00% (v/v)Shea Butter 59.00% (v/v) Vitamin E 0.90% (v/v) Glycerin 15.00% (v/v)Titanium Dioxide 4.00% (w/v) Zinc Oxide 4.00% (w/v) NaOH (pellets) 1.00%(w/v) 2M HCl 5.00% (v/v) Aspen Bark 0.90% (w/v) Sodium Anisate 0.40%(w/v) pH 7

Example 45. Formulation of a Sun Protectant

In an embodiment, a sun protection formulation that may provide a sunprotectant may be:

Water 20.00% (v/v) Hyaluronic Acid 1.00% (w/v) 6% Silk Solution 2.00%(v/v) Coconut Oil 19.00% (v/v) Shea Butter 35.00% (v/v) Vitamin E 0.90%(v/v) Glycerin 20.00% (v/v) Titanium Dioxide 4.00% (w/v) Zinc Oxide4.00% (w/v) NaOH (pellets) 1.60% (w/v) 2M HCl 5.00% (v/v) pH 7

Example 46. Formulation of a Sun Protectant

In an embodiment, a sun protection formulation that may provide a sunprotectant may be:

Water 16.10% (v/v) Hyaluronic Acid 1.50% (w/v) 6% Silk Solution 2.00%(v/v) Coconut Oil 24.00% (v/v) Shea Butter 35.00% (v/v) Vitamin E 0.90%(v/v) Glycerin 10.00% (v/v) Titanium Dioxide 4.00% (w/v) Zinc Oxide4.00% (w/v) NaOH (pellets) 0.8% (w/v) 2M HCl 12.00% (v/v) Aspen Bark0.90% (w/v) Sodium Anisate 0.30% (w/v) pH 6.5

Example 47. Formulation of a Sun Protectant

In an embodiment, a sun protection formulation that may provide a sunprotectant may be:

Water 12.10% (v/v) Hyaluronic Acid 1.00% (w/v) 6% Silk Solution 2.00%(v/v) Coconut Oil 20.00% (v/v) Shea Butter 35.00% (v/v) Raspberry SeedOil 5.00% (v/v) Vitamin E 0.90% (v/v) Glycerin 15.00% (v/v) TitaniumDioxide 3.50% (w/v) Zinc Oxide 3.50% (w/v) NaOH (pellets) 1.00% (w/v) 2MHCl 10.00% (v/v) pH 6.56

Example 48. Formulation of a Sun Protectant

In an embodiment, a sun protection formulation that may provide a sunprotectant may be:

Water 10.10% (v/v) Hyaluronic Acid 1.00% (w/v) 6% Silk Solution 2.00%(v/v) Coconut Oil 25.00% (v/v) Shea Butter 30.00% (v/v) Raspberry SeedOil 10.00% (v/v) Vitamin E 0.90% (v/v) Glycerin 10.00% (v/v) TitaniumDioxide 3.50% (w/v) Zinc Oxide 3.50% (w/v) NaOH (pellets) 75.00% (w/v)2M HCl 12.00% (v/v)

Example 49. Formulation of a Sun Protectant

In an embodiment, a sun protection formulation that may provide a sunprotectant may be:

Water 25.00% (v/v) Hyaluronic Acid 1.00% (w/v) 6% Silk Solution 2.00%(v/v) Coconut Oil 29.00% (v/v) Shea Butter 25.00% (v/v) Raspberry SeedOil 10.00% (v/v) Vitamin E 0.90% (v/v) Glycerin 8.00% (v/v) TitaniumDioxide 1.50% (w/v) Zinc Oxide 6.00% (w/v) NaOH (pellets) 0.10% (w/v) 2MHCl 5.00% (v/v) pH 5.5

Example 50. Formulation of a Sun Protectant

In an embodiment, a sun protection formulation that may provide a sunprotectant may be:

Water 27.50% (v/v) Hyaluronic Acid 1.20% (w/v) 6% Silk Solution 2.00%(v/v) Coconut Oil 30.00% (v/v) Shea Butter 15.60% (v/v) Raspberry SeedOil 12.50% (v/v) Vitamin E 0.90% (v/v) Glycerin 4.00% (v/v) TitaniumDioxide 2.50% (w/v) Zinc Oxide 7.00% (w/v) NaOH (pellets) 0.15% (w/v) 2MHCl 7.50% (v/v) pH 6.00

Example 51. Formulation of a Sun Protectant

In an embodiment, a sun protection formulation that may provide a sunprotectant may be:

Water 30.00% (v/v) Hyaluronic Acid 0.47% (w/v) 6% Silk Solution 2.30%(v/v) Coconut Oil 30.00% (v/v) Shea Butter 13.00% (v/v) Raspberry SeedOil 5.00% (v/v) Vitamin E 0.90% (v/v) Glycerin 6.00% (v/v) TitaniumDioxide 7.14% (w/v) Zinc Oxide 12.00% (w/v) 5N NaOH 0.10% (v/v) 2M HCl10.00% (v/v) Aspen Bark 0.90% (w/v) Sodium Anisate 0.30% (w/v) pH 5-6

Example 52. Formulation of a Sun Protectant

In an embodiment, a sun protection formulation that may provide a sunprotectant may be:

Water 35.00% (v/v) Hyaluronic Acid 0.60% (w/v) 6% Silk Solution 2.00%(v/v) Coconut Oil 30.00% (v/v) Shea Butter 14.00% (v/v) Raspberry SeedOil 5.00% (v/v) Vitamin E 0.90% (v/v) Glycerin 7.00% (v/v) TitaniumDioxide 6.00% (w/v) Zinc Oxide 10.00% (w/v) 5N NaOH 0.10% (v/v) 2M HCl6.00% (v/v) Aspen Bark 0.90% (w/v) Sodium Anisate 0.30% (w/v) pH 6.1

Example 53. An Exemplary Formulation of a Sun Protectant

In an embodiment, a sun protection formulation that may provide a sunprotectant may be:

Water 10-80% (v/v) Hyaluronic Acid 0-5% (w/v) 6% Silk Solution 0.1-20%(v/v) Jojoba Oil 0-60% (v/v) Rosehip Oil 0-60% (v/v) Coconut Oil 0-60%(v/v) Shea Butter 0-60% (v/v) Raspberry Seed Oil 0-60% (v/v) Vitamin E0-10% (v/v) Glycerin 0-80% (v/v) Titanium Dioxide 0-25% (w/v) Zinc Oxide0-25% (w/v) 5N NaOH 0.05-10% (v/v) NaOH (pellets) 0.05-10 2M HCl 0.1-30%(v/v) Aspen Bark 0-5% (w/v) Sodium Anisate 0-5% (w/v)

Example 54. An Exemplary Method for Preparing the Sun ProtectionFormulations of Examples 41 to 53

A solution is first prepared by dissolving or otherwise adding NaOH towater. Where applicable, hyaluronic acid is added to the NaOH solutionand stirred to dissolution. Where applicable, glycerin is also added tothe solution and stirred. Silk is then added. The resulting mixture isthen heated to about 50 to 60° C. with stirring. One or more of coconutoil, vitamin E, jojoba oil, shea butter, and raspberry seed oil arecombined and then heated to about 70° C. with stirring. One or both oftitanium dioxide and zinc oxide are then added to the oil blend andstirred. The combination of the oil blend and oxides are added to theaqueous mixture. The titanium oxide and/or zinc oxide may be added tothe aqueous phase, the oil phase, or both. HCl is then added to thecombined mixture and stirred. Where applicable, aspen bark and/or sodiumanisate is then added with stirring.

Example 55. Formulation of a Stearic Acid Cleanser

In an embodiment, a cleanser formulation that may provide a cleanser maybe:

Water 70.46% (v/v) 6% Silk Solution 1.67% (v/v) Hyaluronic Acid 1.6%(w/v) 5N NaOH 0.15% (v/v) Stearic Acid 10% (v/v) Jojoba Oil 15% (v/v)Aspen Bark 0.90% (w/v) Sodium Anisate 0.30% (w/v) pH 6.03

Example 56. Formulation of a Stearic Acid Cleanser

In an embodiment, a cleanser formulation that may provide a cleanser maybe:

Water 75.40% (v/v) 6% Silk Solution 1.67% (v/v) Hyaluronic Acid 1.6%(w/v) 5N NaOH 0.15% (v/v) Stearic Acid 5% (v/v) Olive Oil 3% (v/v)Jojoba Oil 12% (v/v) Aspen Bark 0.90% (w/v) Sodium Anisate 0.30% (w/v)pH 5.94

Example 57. Formulation of a Stearic Acid Cleanser

In an embodiment, a cleanser formulation that may provide a cleanser maybe:

Water 75.40% (v/v) 6% Silk Solution 1.67% (v/v) Hyaluronic Acid 1.6%(w/v) 5N NaOH 0.15% (v/v) Stearic Acid 5% (v/v) Coconut Oil 15% (v/v)Aspen Bark 0.90% (w/v) Sodium Anisate 0.30% (w/v) pH 6.47

Example 58. An Exemplary Method for Preparing the Stearic Acid Cleansersof Examples 55-57

Dissolve hyaluronic acid in water to prepare a solution and then addsilk slowly.

Refrigerate the solution. Heat a combination of stearic acid, jojobaoil, coconut oil, and/or olive oil to about 75° C. Then, heat thehyaluronic acid/silk solution to about 55° C. Add stearic acid/jojobaoil combination to the hyaluronic acid/silk solution and mix vigorously.To the mixing solution, add NaOH and recover the product cleanser.

Example 59. Formulation of a Lauric Acid Cleanser

In an embodiment, a cleanser formulation that may provide a cleanser maybe:

Water 75.40% (v/v) 6% Silk Solution 1.67% (v/v) Hyaluronic Acid 1.6%(w/v) 5N NaOH 0.15% (v/v) Lauric Acid 2% (v/v) Myristic Acid 2% (v/v)Jojoba Oil 15% (v/v) Aspen Bark 0.90% (w/v) Sodium Anisate 0.30% (w/v)pH 7.17

Example 60. Formulation of a Lauric Acid Cleanser

In an embodiment, a cleanser formulation that may provide a cleanser maybe:

Water 72.85% (v/v) 6% Silk Solution 2.00% (v/v) Hyaluronic Acid 1.75%(w/v) 5N NaOH 0.15% (v/v) Lauric Acid 2.50% (v/v) Stearic Acid 2.50%(v/v) Jojoba Oil 20% (v/v) Aspen Bark 0.90% (w/v) Sodium Anisate 0.30%(w/v) pH 7.26

Example 61. An Exemplary Method for Preparing the Lauric Acid Cleansersof Examples 59 and 60

Dissolve hyaluronic acid in water to prepare a solution and then addsilk slowly. Refrigerate the solution. Heat a combination of lauricacid, jojoba oil, myristic acid, and/or stearic acid to about 75° C.Then, heat the hyaluronic acid/silk solution to about 55° C. Add theacid/jojoba oil combination to the hyaluronic acid/silk solution andmix. Allow the solution to cool and then add aspen bark and sodiumanisate to provide the cleanser.

Example 62. Formulation of a Combination Cleanser

In an embodiment, a cleanser formulation that may provide a cleanser maybe:

Water (v/v) 24.0% 6% Silk Solution (v/v) 10.0% Glycerin (v/v) 20.0% NaOHPellets (w/v) 5.0% Lauric Acid (v/v) 5.0% Myristic Acid (v/v) 20.0%Stearic Acid (v/v) 10.0% Oleic Acid (v/v) 10.0% Aspen Bark (w/v) 0.5%Sodium Anisate (w/v) 0.3% pH 8.38

Example 63. Formulation of a Combination Cleanser

In an embodiment, a cleanser formulation that may provide a cleanser maybe:

Water (v/v) 20.0% 6% Silk Solution (v/v) 10.0% Glycerin (v/v) 25.0% NaOHPellets (w/v) 4.0% Lauric Acid (v/v) 5.0% Myristic Acid (v/v) 10.0%Stearic Acid (v/v) 10.0% Oleic Acid (v/v) 10.0% Jojoba Oil (v/v) 10.0%Aspen Bark (w/v) 0.5% Sodium Anisate (w/v) 0.3% pH 8.42

Example 64. Formulation of a Combination Cleanser

In an embodiment, a cleanser formulation that may provide a cleanser maybe:

Water (v/v) 20.0% 6% Silk Solution (v/v) 15.0% Glycerin (v/v) 30.0% NaOHPellets (w/v) 4.0% Lauric Acid (v/v) 15.0% Oleic Acid (v/v) 15.0% JojobaOil (v/v) 5.0% Aspen Bark (w/v) 0.5% Sodium Anisate (w/v) 0.3% pH 8.42

Example 65. Formulation of a Combination Cleanser

In an embodiment, a cleanser formulation that may provide a cleanser maybe:

Water (v/v) 23.5% 6% Silk Solution (v/v) 5.9% Glycerin (v/v) 14.7% NaOHPellets (w/v) 2.4% Lauric Acid (v/v) 2.9% Myristic Acid (v/v) 5.9%Stearic Acid (v/v) 1.5% Oleic Acid (v/v) 4.4% Squalene Oil (v/v) 11.7%Rosehip Oil (v/v) 26.4% 2M HCl (v/v) 3.22% pH 8.5

Example 66. Formulation of a Combination Cleanser

In an embodiment, a cleanser formulation that may provide a cleanser maybe:

Water (v/v) 25.2% 6% Silk Solution (v/v) 5.8% Glycerin (v/v) 15.0% NaOHPellets (w/v) 2.4% Lauric Acid (v/v) 2.9% Myristic Acid (v/v) 4.5%Stearic Acid (v/v) 1.5% Oleic Acid (v/v) 5.9% Squalene Oil (v/v) 10.0%Lemongrass Oil (v/v) 0.2% 2M HCl (v/v) 3.3% Aspen Bark (w/v) 0.9% SodiumAnisate (w/v) 0.3% pH 8.4

Example 67. Formulation of a Combination Cleanser

In an embodiment, a cleanser formulation that may provide a cleanser maybe:

Water (v/v) 37.8% (20.8% initial, 17% end) 6% Silk Solution (v/v) 4.6%Glycerin (v/v) 12.0% NaOH Pellets (w/v) 2.0% Lauric Acid (v/v) 2.3%Myristic Acid (v/v) 4.7% Stearic Acid (v/v) 1.2% Oleic Acid (v/v) 1.2%Olive Oil (v/v) 33.7% Lemongrass Oil (v/v) 0.2% 2M HCl (v/v) 1.1% AspenBark (w/v) 0.9% Sodium Anisate (w/v) 0.3% pH 8.9

Example 68. Formulation of a Combination Cleanser

In an embodiment, a cleanser formulation that may provide a cleanser maybe:

Water (v/v) 38% (20% initial, 18% end) 6% Silk Solution (v/v) 4.6%Glycerin (v/v) 12.0% NaOH Pellets (w/v) 2.0% Lauric Acid (v/v) 2.0%Myristic Acid (v/v) 4.5% Stearic Acid (v/v) 1.0% Oleic Acid (v/v) 4.0%Olive Oil (v/v) 20.0% Jojoba Oil (v/v) 13.5% Lemongrass Oil (v/v) 0.4%2M HCl (v/v) 1.1% Aspen Bark (w/v) 0.9% Sodium Anisate (w/v) 0.3% pH 8.8

Example 69. Formulation of a Combination Cleanser

In an embodiment, a cleanser formulation that may provide a cleanser maybe:

Water (v/v) 20% (initial), 3.25% (end) 6% Silk Solution (v/v) 4.5%Glycerin (v/v) 15.0% NaOH Pellets (w/v) 2.0% Myristic Acid (v/v) 5.4%Stearic Acid (v/v) 2.1% Oleic Acid (v/v) 4.0% Olive Oil (v/v) 33%(initial), 11% (end) Lemongrass Oil (v/v) 0.2% 2M HCl (v/v) 1.3% AspenBark (w/v) 0.9% Sodium Anisate (w/v) 0.3% pH 8.75

Example 70. An Exemplary Method for Preparing the Combination Cleansersof Examples 62 and 69

Heat lauric acid, stearic acid, myristic acid, oleic acid, squalene oil,rosehip oil, lemongrass oil, olive oil, and/or jojoba oil to about 75°C. Then dissolve NaOH in water (or an initial aliquot of water) and heatthe solution to about 70° C. To the NaOH solution add glycerin and silk,then add the blend of lauric acid, stearic acid, myristic acid, oleicacid, squalene oil, rosehip oil, lemongrass oil, olive oil, and/orjojoba oil. Allow the mixture to cool. Where applicable, reheat themixture and add rosehip oil, squalene oil, and/or 2M HCl. Then, whereapplicable, add an ending aliquot of water and/or olive oil. Finally,add aspen bark and/or sodium anisate to yield the combination cleanser.

Example 71. Formulation of a Cleansing Silk Refresh Product

In an embodiment, a cleanser formulation that may provide a cleansingsilk refresh product may be:

Water (v/v) 34.66% (18% initial, 16.66% end) 6% Silk Solution (v/v)4.60% Glycerin (v/v) 11.80% NaOH pellets (w/v) 2.00% Lauric Acid (v/v)2.56% Myristic Acid (v/v) 5.30% Stearic Acid (v/v) 1.38% Oleic Acid(v/v) 3.60% Olive Oil (v/v) 33.00% Lemongrass Oil (v/v) 2M HCl (v/v)1.10% Aspen Bark(w/v) 0.90% Sodium Anisate (w/v) 0.30% pH 9.25

Example 72. Formulation of a Cleansing Silk Refresh Product

In an embodiment, a cleanser formulation that may provide a cleansingsilk refresh product may be:

Water (v/v) 34.7% (18% initial, 16.7% end) 6% Silk Solution (v/v) 4.60%Glycerin (v/v) 11.80% NaOH pellets (w/v) 2.00% Lauric Acid (v/v)Myristic Acid (v/v) 6.58% Stearic Acid (v/v) 2.66% Oleic Acid (v/v)3.60% Olive Oil (v/v) 33.00% Lemongrass Oil (v/v) 0.20% 2M HCl (v/v)1.10% Aspen Bark(w/v) 0.90% Sodium Anisate (w/v) 0.30% pH 9.5

Example 73. Formulation of a Cleansing Silk Refresh Product

In an embodiment, a cleanser formulation that may provide a cleansingsilk refresh product may be:

Water (v/v) 40% (21.8% initial, 18.2% end) 6% Silk Solution (v/v) 1.00%Glycerin (v/v) 11.80% NaOH pellets (w/v) 2.00% Lauric Acid (v/v) 2.56%Myristic Acid (v/v) 5.30% Stearic Acid (v/v) 1.38% Oleic Acid (v/v)3.60% Olive Oil (v/v) 33.00% Lemongrass Oil (v/v) 0.20% 2M HCl (v/v)2.00% Aspen Bark(w/v) 0.90% Sodium Anisate (w/v) pH 8.92

Example 74. Formulation of a Cleansing Silk Refresh Product

In an embodiment, a cleanser formulation that may provide a cleansingsilk refresh product may be:

Water (v/v) 41.36% (21.36% initial, 19% end) 6% Silk Solution (v/v)1.00% Glycerin (v/v) 11.80% NaOH pellets (w/v) 2.00% Lauric Acid (v/v)Myristic Acid (v/v) 6.58% Stearic Acid (v/v) 2.66% Oleic Acid (v/v)3.60% Olive Oil (v/v) 33.00% Lemongrass Oil (v/v) 2M HCl (v/v) 4.00%Aspen Bark(w/v) Sodium Anisate (w/v) pH 8.8

Example 75. Formulation of a Cleansing Silk Refresh Product

In an embodiment, a cleanser formulation that may provide a cleansingsilk refresh product may be:

Water (v/v) 38.6% (20% initial, 18.36% end) 6% Silk Solution (v/v) 1.00%Glycerin (v/v) 11.80% NaOH pellets (w/v) 2.00% Lauric Acid (v/v) 2.56%Myristic Acid (v/v) 5.30% Stearic Acid (v/v) 1.38% Oleic Acid (v/v)3.60% Olive Oil (v/v) 33.00% Lemongrass Oil (v/v) 2M HCl (v/v) 3.00%Aspen Bark(w/v) 0.90% Sodium Anisate (w/v) 0.40% pH 9.06

Example 76. Formulation of a Cleansing Silk Refresh Product

In an embodiment, a cleanser formulation that may provide a cleansingsilk refresh product may be:

Water (v/v) 36.16% (19% initial, 17.16% end) 6% Silk Solution (v/v)1.00% Glycerin (v/v) 12.00% NaOH pellets (w/v) 2.00% Lauric Acid (v/v)2.56% Myristic Acid (v/v) 5.30% Stearic Acid (v/v) 1.38% Oleic Acid(v/v) 3.60% Olive Oil (v/v) 33.00% Lemongrass Oil (v/v) 2M HCl (v/v)5.00% Aspen Bark(w/v) Sodium Anisate (w/v) 0.50% pH 8.5

Example 77. An Exemplary Method for Preparing the Cleansing Silk RefreshProducts of Examples 71 and 76

Heat applicable acids, lemongrass oil, and/or olive oil to 75° C.Dissolve NaOH in an initial aliquot of water and heat the solution to70° C. To the alkaline solution add glycerin and silk solution, then addthe blend of applicable acids, lemongrass oil, and/or olive oil. Allowthe mixture to cool and then add 2M HCl followed by an ending aliquot ofwater. Where applicable, then add the aspen bark and/or the sodiumanisate.

Example 78. Formulation of a Cleansing Silk Complete Product

In an embodiment, a cleanser formulation that may provide a cleansingsilk complete product may be:

Water (v/v) 17.5% (initial), 2.95% (end) 6% Silk (v/v) 4.5% Glycerin(v/v) 15.0% NaOH pellets (w/v) 2.0% Myristic Acid (v/v) 6.3% StearicAcid (v/v) 2.5% Oleic Acid (v/v) 4.0% Olive Oil (v/v) 33% (initial), 11%(end) Lemongrass Oil (v/v) 0.2% 2M HCl (v/v) 3.3% Aspen Bark(w/v) 0.9%Sodium Anisate (w/v) 0.3% pH 8.76

Example 79. Formulation of a Cleansing Silk Complete Product

In an embodiment, a cleanser formulation that may provide a cleansingsilk complete product may be:

Water (v/v) 17.75% (initial), 2.5% (end) 6% Silk (v/v) 4.5% Glycerin(v/v) 15.0% NaOH pellets (w/v) 2.0% Myristic Acid (v/v) 6.3% StearicAcid (v/v) 2.5% Oleic Acid (v/v) 4.0% Olive Oil (v/v)  33% (initial),11% (end) Lemongrass Oil (v/v) 0.2% 2M HCl (v/v) 3.3% Aspen Bark(w/v)0.9% Sodium Anisate (w/v) 0.3%

Example 80. Formulation of a Cleansing Silk Complete Product

In an embodiment, a cleanser formulation that may provide a cleansingsilk complete product may be:

Water (v/v) 17.75% (initial), 2.5% (end) 6% Silk (v/v) 4.5% Glycerin(v/v) 15.0% NaOH pellets (w/v) 2.0% Myristic Acid (v/v) 6.3% StearicAcid (v/v) 2.5% Oleic Acid (v/v) 4.0% Olive Oil (v/v)  33% (initial),11% (end) Lemongrass Oil (v/v) 0.2% 2M HCl (v/v) 3.3% Aspen Bark(w/v)0.9% Sodium Anisate (w/v) 0.3% pH 8.8

Example 81. Formulation of a Cleansing Silk Complete Product

In an embodiment, a cleanser formulation that may provide a cleansingsilk complete product may be:

Water (v/v) 17.75% (initial), 2.5% (end) 6% Silk (v/v) 4.5% Glycerin(v/v) 15.0% NaOH pellets (w/v) 2.0% Myristic Acid (v/v) 6.3% StearicAcid (v/v) 2.5% Oleic Acid (v/v) 4.0% Olive Oil (v/v)  33% (initial),11% (end) Lemongrass Oil (v/v) 0.2% 2M HCl (v/v) 3.3% Aspen Bark(w/v)Sodium Anisate (w/v) pH 8.98

Example 82. Formulation of a Cleansing Silk Complete Product

In an embodiment, a cleanser formulation that may provide a cleansingsilk complete product may be:

Water (v/v) 17.75% (initial), 2.5% (end) 6% Silk (v/v) 4.5% Glycerin(v/v) 15.0% NaOH pellets (w/v) 2.0% Myristic Acid (v/v) 6.3% StearicAcid (v/v) 2.5% Oleic Acid (v/v) 4.0% Olive Oil (v/v)  33% (initial),11% (end) Lemongrass Oil (v/v) 0.2% 2M HCl (v/v) 3.3% Aspen Bark(w/v)Sodium Anisate (w/v) pH 8.98

Example 83. Formulation of a Cleansing Silk Complete Product

In an embodiment, a cleanser formulation that may provide a cleansingsilk complete product may be:

Water (v/v) 20.2% (initial), 5% (end) 6% Silk (v/v) 1.00% Glycerin (v/v)15.00% NaOH pellets (w/v) 2.00% Myristic Acid (v/v) 6.25% Stearic Acid(v/v) 2.50% Oleic Acid (v/v) 4.00% Olive Oil (v/v)   33% (initial), 11%(end) Lemongrass Oil (v/v) 2M HCl (v/v) 3.30% Aspen Bark(w/v) SodiumAnisate (w/v) 0.30% pH 8.82

Example 84. An Exemplary Method for Preparing the Cleansing SilkComplete Products of Examples 79 and 83

Heat applicable acids, olive oil (an initial aliquot), and/or lemongrassoil to about 75° C. Dissolve NaOH in an initial aliquot of water andheat the solution to 70° C. To the alkaline solution add glycerin andsilk solution, then add the blend of applicable acids, lemongrass oil,and/or olive oil. Allow the mixture to cool and then add 2M HCl followedby ending aliquots of water and olive oil. Where applicable, then addaspen bark and and/or sodium anisate.

Example 85. An Exemplary Cleansing Silk Refresh Formulation

In an embodiment, a cleanser formulation that may provide a cleansingsilk refresh product may include:

Water (v/v) 10-60% (total of initial and ending aliquots) 6% Silk (v/v)0.1-20%  Glycerin (v/v) 0-50% NaOH pellets (w/v) 0.1-5%  Lauric Acid(v/v) 0-10% Myristic Acid (v/v) 0-20% Stearic Acid (v/v)  0-5% OleicAcid (v/v) 0-10% Olive Oil (v/v) 5-50% 2M HCl (v/v) Sodium Anisate (w/v)0.1-5%  pH 8 to 9

Example 86. An Exemplary Cleansing Silk Complete Formulation

In an embodiment, a cleanser formulation that may provide a cleansingsilk complete product may include:

Water (v/v) 10-40% (total of initial and ending aliquots) 6% Silk (v/v)0.1-20%  Glycerin (v/v) 0-50% NaOH pellets (w/v) 0.1-5%  Myristic Acid(v/v) 0-20% Stearic Acid (v/v)  0-5% Oleic Acid (v/v) 0-10% Olive Oil(v/v) 10-75%  Sodium Anisate (w/v) 0.1-5%  pH 8 to 9

Example 87. Microbial and Fungal Challenge Testing for Cleansing Agents

The formulations of Examples 71, 72, 73, 75, 76, 78, 80, and 81 weretested to determine their anti-microbial and anti-fungal activities.Each of the tested formulations was found to have anti-bacterial andanti-fungal properties. Each of these tested formulations passedantibacterial and antifungal challenge testing specified in ISO standardISO 11930.

Example 88. Patch (Sensitivity) Testing for Cleansing Agents

The formulations of Examples 71, 72, 73, 75, 76, 78, 80, and 81 weretested for irritation and sensitization by Repeated Insult PatchTesting. Each tested formulation was considered a non-primary irritantand non-primary sensitizer confirmed by a dermatologist.

Example 89. Shelf Life Testing for Cleansing Agents

The formulations of Examples 71, 72, 78, 80, and 81 were tested todetermine their shelf life. The cleansers of the formulations wereplaced in a 40° C. incubator to test time stability. The time stabilityresults are provided below:

Cleanser Formulation Test Result Example 78 Over 4.5 months withoutphase separation Example 80 Over 4 months without phase separationExample 81 Over 4 months without phase separation Example 71 Phaseseparation at 4 months Example 72 Over 4 months without phase separation

Example 90. An Exemplary Moisturizer Formulation

In an embodiment, a moisturizer formulation that may provide ahyaluronic acid free moisturizer may include:

Water (v/v) 10.0% 6% Silk (v/v) 10.00% Glycerin (v/v) 55.00% NaOHpellets (w/v) 2.00% Coconut Oil 10.00% Vitamin E 0.90% Shea Butter10.00% 2M HCl (v/v) 3.30% Aspen Bark(w/v) 0.90% Sodium Anisate (w/v)0.30% pH 5 to 8.5

Example 91. An Exemplary Method for Preparing the Moisturizer of Example90

The glycerin, silk solution, and NaOH may be added to water and heatedto about 70° C. Vitamin E, coconut oil, and shea butter may be heated toabout 70° C. The oils may be then be added to the glycerin and silksolution under vigorous stirring while heating. The mixture may beallowed to cool. Then 2M HCl, aspen bark, and sodium anisate may beadded to produce the moisturizer.

Example 92. Formulation of a Deodorant Base Product

In an embodiment, a deodorant formulation that may provide a deodorantbase product may be:

Water (v/v) 5.00%   6% silk solution (v/v) 0.30%   Beeswax (w/v) 34% Coconut Oil (w/v) 28.00%    Shea Butter (w/v) 20%  Glycerin (v/v) 5%Sunflower Oil (v/v) 2% Vitamin E Oil (v/v) 2%

Example 93. An Exemplary Formulation of a Deodorant Base Product

In an embodiment, a deodorant formulation that may provide a deodorantbase product may include:

Water (v/v) 1-20% 6% silk solution (v/v) 0.1-5%  Beeswax (w/v) 10-50% Coconut Oil (w/v) 0-40% Shea Butter (w/v) 0-60% Glycerin (v/v) 0-15%Sunflower Oil (v/v) 0-10% Vitamin E Oil (v/v)  0-5% Preservative (w/v)(e.g., aspen bark, 0.1-5%  sodium anisate, glyceryl caprylate, sodiumphytate)

Example 94. An Exemplary Formulation of a Deodorant or AntiperspirantProduct

In an embodiment, a deodorant or antiperspirant formulation of theinvention may include:

Aluminum based compounds (w/v) up to 25% Mineral Salts (includingaluminum) (w/v) up to 25% Talcum Powder (w/v) up to 20% Sodiumbicarbonate (w/v) up to 20% Sodium stearate (w/v) up to 20% Witch Hazel(v/v) up to 20% Baking Soda (w/v) up to 20% Hops (w/v) up to 20% AloeVera (w/v) up to 10% Essential Oils (v/v) up to 10%(antibacterial/antifungal properties)

Example 95. Formulation of a Foot Balm

In an embodiment, a foot balm formulation that may provide a foot balmproduct may include:

Water (v/v) 5.00%   6% silk solution (v/v) 0.30%   Beeswax (w/v) 34% Coconut Oil (w/v) 28.00%    Shea Butter (w/v) 20%  Glycerin (v/v) 5%Sunflower Oil (v/v) 2% Vitamin E Oil (v/v) 2% Preservative (w/v) (e.g.,aspen bark, sodium anisate, glyceryl caprylate, sodium phytate)Antimicrobial essential oil (v/v) 2% (e.g., lemongrass oil, eucalyptusoil, tea tree oil, rosemary oil)

Example 96. An Exemplary Formulation of a Foot Balm

In an embodiment, an exemplary foot balm formulation that may provide afootbalm product may include:

Water (v/v) 1-20% 6% silk solution (v/v) 0.1-5%  Beeswax (w/v) 10-50% Coconut Oil (w/v) 0-40% Shea Butter (w/v) 0-60% Glycerin (v/v) 0-15%Sunflower Oil (v/v) 0-10% Vitamin E Oil (v/v)  0-5% Preservative (w/v)(e.g., aspen bark, 0.1-5%  sodium anisate, glyceryl caprylate, sodiumphytate) Antimicrobial essential oil (v/v)  0-2% (e.g., lemongrass oil,eucalyptus oil, tea tree oil, rosemary oil)

Example 97. Formulation of a Shampoo

In an embodiment, a shampoo formulation that may provide a shampooproduct may include:

Water (v/v) 40% 6% Silk (v/v) 2% Glycerin (v/v) 10% NaOH pellets (w/v)2% Lauric Acid (v/v) 3% Myristic Acid (v/v) 7% Stearic Acid (v/v) 3%Oleic Acid (v/v) 17% Olive Oil (v/v) 9% 2M HCl (v/v) 5% Sodium Anisate(w/v) 1% Essential Oils (v/v) 1%

Example 98. Formulation of a Shampoo

In an embodiment, a shampoo formulation that may provide a shampooproduct may include:

Water (v/v) 40% 6% Silk (v/v) 2% Glycerin (v/v) 10% NaOH pellets (w/v)2% Sodium Lauryl/Laureth Sulfate (v/v) 30% (e.g., ammonium laurylsulfate) Olive Oil (v/v) 9% 2M HCl (v/v) 5% Sodium Anisate (w/v) 1%Essential Oils (v/v) 1%

Example 99. An Exemplary Formulation of a Shampoo

In an embodiment, an exemplary shampoo formulation that may provide ashampoo product may include:

Water (v/v) 5 to 75% 6% Silk (v/v) 0.1-20%   Glycerin (v/v) 0-50% NaOHpellets (w/v) 0.1-5%   Lauric Acid (v/v) 0-10% Myristic Acid (v/v) 0-20%Stearic Acid (v/v) 0-5%  Oleic Acid (v/v) 0-30% Olive Oil (v/v) 5-40% 2MHCl (v/v) Sodium Anisate (w/v) 0.1-5%   Essential Oils (v/v) 0.1-20%  

Example 100. An Exemplary Formulation of a Shampoo

In an embodiment, an exemplary shampoo formulation that may provide ashampoo product may include:

Water (v/v) 5 to 75% 6% Silk (v/v) 0.1-20%   Glycerin (v/v) 0-50% NaOHpellets (w/v) 0.1-5%   Sodium Lauryl/Laureth Sulfate (v/v) 0-50% OliveOil (v/v) 5-40% 2M HCl (v/v) Sodium Anisate (w/v) 0.1-5%   EssentialOils (v/v) 0.1-20%  

Example 101. Formulation of a Conditioner

In an embodiment, a conditioner formulation that may provide aconditioner product may include:

Water (v/v) 78%  6% Silk (v/v) 2% Hyaluronic Acid (w/v) 1.4%   Glycerin(v/v) 2% NaOH pellets (w/v) 2% Stearic Acid (v/v) 3% Oleic Acid (v/v) 7%Olive Oil (v/v) 5% 2M HCl (v/v) 4% Sodium Anisate (w/v) 1% EssentialOils (v/v) 1%

Example 102. An Exemplary Formulation of a Conditioner

In an embodiment, an exemplary conditioner formulation that may providea conditioner product may include:

Water (v/v) 40-95%  6% Silk (v/v) 0.1-20%   Hyaluronic Acid (w/v)0.5-5%   Glycerin (v/v) 0-50% NaOH pellets (w/v) 0.1-5%   Stearic Acid(v/v) 0-10% Oleic Acid (v/v) 0-20% Olive Oil (v/v) 5-40% 2M HCl (v/v)Sodium Anisate (w/v) 0.1-5%   Essential Oils (v/v) 0.1%-20%  

Example 103. Formulation of a Lip Balm

In an embodiment, a lip balm formulation that may provide a lip balmproduct may be:

Water (v/v) 9.40% 6% silk solution (v/v) 0.60% Beeswax (v/v) 27.50%Coconut Oil (v/v) 37.50% Shea Butter (v/v) 18.50% Sweet Orange EssentialOil (v/v) 0.50% Sunflower Oil (v/v) 5.00% Vitamin E Oil (v/v) 1.00%

Example 104. Method of Manufacturing the Lip Balm of Example 103

Vitamin E, sunflower oil, and sweet orange oil were heated in one beakerto about 70° C. Coconut oil, shea butter, and beeswax was melted atabout 75° C. The two mixtures were combined under heating at about 80°C. To the mixture was added silk solution under vigorous stirring atabout 35° C. Poured heated mixture into mold or tube at room temperatureand placed in an oven at 50° C. for about 15 minutes. Then, placedfilled mold or tube into a 35° C. oven for about 15 minutes. The filledmold or tube was then allowed to stand at room temperature until hard.

Example 105. Formulation of a Lip Balm

In an embodiment, a lip balm formulation that may provide a lip balmproduct may be:

Water (v/v) 4.70% 6% silk solution (v/v) 0.30% Beeswax (w/v) 34.00%Coconut Oil (w/v) 28.85% Shea Butter (w/v) 19.00% Glycerin (v/v) 5.00%Sunflower Oil (v/v) 5.00% Vitamin E Oil (v/v) 2.50% Dermofeel PA-3 (v/v)0.20% Spearmint Essential Oil (v/v) 0.15% Peppermint Essential Oil (v/v)0.30%

Example 106. Formulation of a Lip Balm

In an embodiment, a lip balm formulation that may provide a lip balmproduct may be:

Water (v/v) 4.70% 6% silk solution (v/v) 0.30% Beeswax (w/v)   34%Coconut Oil (w/v) 28.85%  Shea Butter (w/v)   19% Glycerin (v/v)   5%Sunflower Oil (v/v)  2.7% Vitamin E Oil (v/v) 1.00% Glyceryl Caprylate(w/v) 4.00% Spearmint Essential Oil (v/v) 0.15% Peppermint Essential Oil(v/v) 0.30%

Example 107. Formulation of a Lip Balm

In an embodiment, a lip balm formulation that may provide a lip balmproduct may be:

Water (v/v) 4.70% 6% silk solution (v/v) 0.30% Beeswax (w/v)   34%Coconut Oil (w/v) 28.85%  Shea Butter (w/v)   19% Glycerin (v/v)   5%Sunflower Oil (v/v)   5% Vitamin E Oil (v/v) 1.75% Glyceryl Caprylate(w/v) 0.95% Spearmint Essential Oil (v/v) 0.15% Peppermint Essential Oil(v/v) 0.30%

Example 108. Formulation of a Lip Balm

In an embodiment, a lip balm formulation that may provide a lip balmproduct may be:

Water (v/v) 4.70% 6% silk solution (v/v) 0.30% Beeswax (w/v)   34%Coconut Oil (w/v) 28.85%  Shea Butter (w/v)   19% Glycerin (v/v)   5%Sunflower Oil (v/v)   5% Vitamin E Oil (v/v) 2.20% Glyceryl Caprylate(w/v) 0.50% Spearmint Essential Oil (v/v) 0.15% Peppermint Essential Oil(v/v) 0.30%

Example 109. An Exemplary Formulation of a Lip Balm

In an embodiment, a lip balm formulation that may provide a lip balmproduct may include:

Water (v/v) 4.70% 6% silk solution (v/v) 0.30% Beeswax (w/v) 31.40%Coconut Oil (w/v) 31.40% Shea Butter (w/v) 17.85% Glycerin (v/v) 5.00%Sunflower Oil (v/v) 6.00% Vitamin E Oil (v/v) 2.40% Glyceryl Caprylate(w/v) 0.50% Essential Oil (v/v) (e.g., 0.45% spearmint oil, peppermintoil)

Example 110. An Exemplary Formulation of a Lip Balm

In an embodiment, a lip balm formulation that may provide a lip balmproduct may include:

Water (v/v) 0.1-25%  6% silk solution (v/v) 0.01-1.6%  Beeswax (w/v)20-50% Coconut Oil (w/v) 10-50% Shea Butter (w/v) 10-50% Glycerin (v/v) 0-20% Sunflower Oil (v/v)  0-20% Vitamin E Oil (v/v)  0-20% GlycerylCaprylate (w/v) 0-5% Spearmint Essential Oil (v/v) 0-3% PeppermintEssential Oil (v/v)  0-25% pH 5 to 6

Example 111. Method of Manufacturing the Lip Balms of Examples 105 to110

In one beaker, vitamin E, beeswax, shea butter, coconut oil, andessential oils are combined. The mixture is then heated to about 75° C.In a covered glass beaker, glycerin, silk solution and gyceryl caprylateare combined and heated to about 70° C. The mixture of oils are thenadded into the aqueous solution and mixed under heating at about 75° C.for about 10 minutes. The heated mixture is then poured into a mold ortube at room temperature to provide the lip balm product. Once filledand semi-hard, additional heated mixture is poured over top of the moldor tube to provide a smoother top.

Example 112. Lip Balm Stability Study

Certain lip exemplary lip balms of the invention were tested todetermine their stability over a period of days. Stability wasdetermined by examining the lip balm products. Lip balm stability isindicated in the table below:

Formulation Days stable Example 103 161 Example 105 134 Example 106 111Example 107 111 Example 108 111

Example 113. Lip Balm Thermal Stress Test

Two exemplary lip balm products were placed in a 40° C. incubator and a60° C. incubator, with their caps off, to see if they would melt. Oneweek later, none of the tubes showed any signs of stress. At the 3 weektime point, all of the 40° C. lip balm products showed no signs ofchange. The 60° C. lip balm products had a very small amount of liquidmelted, a slight darkening in color (from off white to light beige) andhad some brown spots/solid-crust (speculated to be vitamin E). The 40°C. lip balm products were then frozen at about −20° C. for two days andthawed without showing signs of stress. The purpose of this test was toensure the lip balm products would not melt at temperatures consumersmight subject them to for short periods of time.

Example 114. Lip Balm Microbial Challenge Testing

Lip balm products of the invention were tested to determine theiranti-fungal and anti-bacterial properties. Each of these testedformulations passed anti-bacterial and anti-fungal challenge testingspecified in ISO standard ISO 11930, with the exception of Example 103.Examples 103, 105, 106, 107, and 108 were tested as shown below:

Formulation Result Example 103 Failed bacteria and fungi Example 105Passed bacteria and fungi Example 106 Passed bacteria and fungi Example107 Passed bacteria and fungi Example 108 Passed bacteria and fungi

All patents, patent applications, and published references cited hereinare hereby incorporated by reference in their entirety. While themethods of the present disclosure have been described in connection withthe specific embodiments thereof, it will be understood that it iscapable of further modification. Further, this application is intendedto cover any variations, uses, or adaptations of the methods of thepresent disclosure, including such departures from the presentdisclosure as come within known or customary practice in the art towhich the methods of the present disclosure pertain.

It will be appreciated by those skilled in the art that changes could bemade to the exemplary embodiments shown and described above withoutdeparting from the broad inventive concepts thereof. It is understood,therefore, that this invention is not limited to the exemplaryembodiments shown and described, but it is intended to covermodifications within the spirit and scope of the present invention asdefined by the claims. For example, specific features of the exemplaryembodiments may or may not be part of the claimed invention and variousfeatures of the disclosed embodiments may be combined. Unlessspecifically set forth herein, the terms “a”, “an” and “the” are notlimited to one element but instead should be read as meaning “at leastone”.

It is to be understood that at least some of the figures anddescriptions of the invention have been simplified to focus on elementsthat are relevant for a clear understanding of the invention, whileeliminating, for purposes of clarity, other elements that those ofordinary skill in the art will appreciate may also comprise a portion ofthe invention. However, because such elements are well known in the art,and because they do not necessarily facilitate a better understanding ofthe invention, a description of such elements is not provided herein.

Further, to the extent that the methods of the present invention do notrely on the particular order of steps set forth herein, the particularorder of the steps should not be construed as limitation on the claims.Any claims directed to the methods of the present invention should notbe limited to the performance of their steps in the order written, andone skilled in the art can readily appreciate that the steps may bevaried and still remain within the spirit and scope of the presentinvention.

1. A composition comprising: about 0.0001% to about 90% (w/v) of puresilk fibroin-based protein fragments that are substantially devoid ofsericin, about 0.1% to about 99% (v/v) of an oil, and about 99% to about0.1% (v/v) water; wherein the pH of the composition is in the range of 4to 9, wherein the composition forms a stable emulsion, wherein the puresilk fibroin-based protein fragments have an average weight averagemolecular weight ranging from about 5 kDa to about 80 kDa, and whereinthe pure silk fibroin-based protein fragments have a polydispersity ofbetween about 1.5 and about 3.0.
 2. The composition of claim 1,comprising about 0.01% to about 2% (w/v) of the pure silk fibroin-basedprotein fragments.
 3. The composition of claim 1, comprising about 0.05%to about 0.3% (w/v) of the pure silk fibroin-based protein fragments. 4.The composition of claim 1, wherein the pH of the composition is in therange of 5 to
 8. 5. The composition of claim 1, wherein the pH of thecomposition is in the range of 5 to
 7. 6. The composition of claim 1,comprising about 0.1% to about 25% of an oil, and about 99% to about 75%water.
 7. The composition of claim 1, comprising about 25% to about 50%of an oil, and about 75% to about 50% water.
 8. The composition of claim1, comprising about 50% to about 75% of an oil, and about 50% to about25% water.
 9. The composition of claim 1, comprising about 75% to about99% of an oil, and about 25% to about 0.1% water.
 10. The composition ofclaim 1, wherein the pure silk fibroin-based protein fragments have anaverage weight average molecular weight ranging from about 5 kDa toabout 18 kDa.
 11. The composition of claim 1, wherein the pure silkfibroin-based protein fragments have an average weight average molecularweight ranging from about 17 kDa to about 40 kDa.
 12. The composition ofclaim 1, wherein the pure silk fibroin-based protein fragments have anaverage weight average molecular weight ranging from about 39 kDa toabout 80 kDa.
 13. The composition of claim 1, further comprising about0.1% to about 8% (w/v) of hyaluronic acid.
 14. The composition of claim1, further comprising about 0.5% to about 2% (w/v) of hyaluronic acid.15. The composition of claim 1, wherein the stable emulsion is selectedfrom the group consisting of a water-in-oil (w/o) emulsion and anoil-in-water (o/w) emulsion.
 16. The composition of claim 1, wherein thecomposition is in a form selected from the group consisting of a liquid,semisolid, solid, lotion, cream, oil, gel, emulsion, stick, sprayointment, paste, mousse, foam, and suspension.
 17. The composition ofclaim 1, wherein the oil is selected from the group consisting of analiphatic oil, a fatty alcohol, a fatty acid, a glyceride (anacylglycerol), a phospholipid, and combinations thereof.
 18. Thecomposition of claim 17, wherein the oil is a glyceride, and theglyceride is selected from the group consisting of a monoglyceride, adiglyceride, and a triglyceride.
 19. The composition of claim 1, whereinthe oil comprises one or more natural or essential oils.
 20. Thecomposition of claim 1, further comprising about 0.1% to about 25% of asecond oil.
 21. The composition of claim 20, wherein the second oilcomprises one or more natural or essential oils.
 22. The composition ofclaim 1, further comprising about 0.1% to about 5% (w/v) or (v/v) of apH adjusting agent.
 23. The composition of claim 22, wherein the pHadjusting agent is selected from the group consisting of sodiumhydroxide (NaOH), potassium hydroxide (KOH), hydrochloric acid (HCl),citric acid, and combinations thereof.
 24. The composition of claim 22,further comprising about 0.1% to about 5% (w/v) or (v/v) of a second pHadjusting agent.
 25. The composition of claim 24 wherein the second pHadjusting agent is selected from the group consisting of sodiumhydroxide (NaOH), potassium hydroxide (KOH), hydrochloric acid (HCl),citric acid, and combinations thereof.
 26. The composition of claim 24,wherein the first pH adjusting agent is sodium hydroxide (NaOH) and thesecond pH adjusting agent is hydrochloric acid (HCl).
 27. Thecomposition of claim 1, further comprising an additive.
 28. Thecomposition of claim 27, wherein the additive is selected from the groupconsisting of vitamin E, vitamin A, vitamin B, vitamin C, aspen bark,sodium anisate, oat flour, titanium oxide, titanium dioxide, glycerin,zinc oxide, a preservative, an aluminum based compound, a mineral salt,talcum powder, sodium bicarbonate, hops, aloe vera, witch hazel, andcombinations thereof.
 29. The composition of claim 28, wherein theadditive is a combination of vitamin E, aspen bark, and sodium anisate.30. The composition of claim 1, further comprising a sunscreen orsunblock.
 31. The composition of claim 30, wherein the sunscreen orsunblock is selected from the group consisting of amiloxate(isopentyl-4-methoxycinnamate), para-aminobenzoic acid, Benzophenone-9(sodium dihydroxy dimethoxy di sulfobenzophenone), padimate O(octyldimethyl para-aminobenzoic acid), phenylbenzimidazole sulfonicacid, cinoxate, dioxybenzone, oxybenzone, homosalate, menthylanthranilate, 4-methylbenzylidene camphor, Mexoryl XL (drometrizoletrisiloxane), Neo Heliopan AP (disodium phenyl dibenzimidazoletetrasulfonate), octocrylene, octyl methoxycinnamate, octyl salicylate,sulisobenzone, Tinosorb M (bisoctrizole, methylene bis-benzotriazolyltetramethylbutylphenol), titanium dioxide, zinc oxide, micronizedtitanium dioxide, micronized zinc oxide, oil soluble zinc oxide,Tinosorb S (bis-ethylhexyloxyphenol methoxyphenol triazine), Tinsorb A2B(tris-biphenyl triazine), trolamine salicylate, avobenzone, ecamsule,titanium dioxide, 4-MBC, Uvinul T 150 (octyl triazone), Uvinul A Plus(diethylamino hydroxybenzoyl hexyl benzoate), Parsol SLX(dimethico-diethylbenzalmalonate), zinc oxide, melanin, a melaninderivative, raspberry seed oil, carrot oil, and combinations thereof.32. The composition of claim 31, wherein the sunscreen or sunblock isselected from the group consisting of titanium dioxide, zinc oxide,micronized titanium dioxide, micronized zinc oxide, oil soluble zincoxide, octylcrylene, avobenzone, octinoxate, octisalate, oxybenzone,homosalate, helioplex, 4-MBC, mexoryl SX and SL, tinosorb S and M,uvinul T 150, uvinul A plus, and a combination thereof.
 33. Thecomposition of claim 1, wherein the composition comprises an emollient.34. The composition of claim 33, wherein the emollient comprises one ormore of a hydrocarbon oil, a hydrocarbon wax, a silicone oil, anacetoglyceride ester, an ethoxylated glyceride, an alkyl ester of afatty acid, an alkenyl ester of a fatty acid, a fatty acid, a fattyalcohol, a fatty alcohol ether, an ether-ester, lanolin, a lanolinderivative, a polyhydric alcohol, a polyether derivative, a polyhydricester, a wax ester, a beeswax derivative, a vegetable wax, a natural oressential oil, a phospholipid, a sterol, and an amide.
 35. Thecomposition of claim 1, wherein the composition is in the form of asunscreen, a cleanser, a bar of soap, a lip balm, a foot balm, adeodorant stick, an antiperspirant stick, a liquid deodorant, a spraydeodorant, a liquid antiperspirant, a spray antiperspirant, aconditioner, a shampoo, or a combination thereof.
 36. A method forpreparing a composition comprising the steps of: providing a compositioncomprising: about 0.0001% to about 90% (w/v) of pure silk fibroin-basedprotein fragments that are substantially devoid of sericin, about 99% toabout 0.1% (v/v) of water; adding a first pH adjusting agent to adjustthe pH of the composition to at least 10; adding about 0.1% to about 99%(v/v) of an oil; mixing the composition until it is homogeneous; addinga second pH adjusting agent to adjust the pH of the composition to therange of 4 to 9; and storing the composition for a period of time,wherein the composition remains a stable emulsion; wherein the pure silkfibroin-based protein fragments have an average weight average molecularweight ranging from about 5 kDa to about 80 kDa, and wherein the puresilk fibroin-based protein fragments have a polydispersity of betweenabout 1.5 and about 3.0.
 37. The method of claim 36, wherein the puresilk fibroin-based protein fragments have an average weight averagemolecular weight ranging from about 5 kDa to about 18 kDa.
 38. Themethod of claim 36, wherein the pure silk fibroin-based proteinfragments have an average weight average molecular weight ranging fromabout 17 kDa to about 40 kDa.
 39. The method of claim 36, wherein thepure silk fibroin-based protein fragments have an average weight averagemolecular weight ranging from about 39 kDa to about 80 kDa.
 40. Themethod of claim 36, further comprising the step of adding 0.1% to 8%(w/v) hyaluronic acid.
 41. The method of claim 36, further comprisingabout 0.1% to about 8% (w/v) of hyaluronic acid.
 42. The method of claim36, wherein the stable emulsion is selected from the group consisting ofa water-in-oil (w/o) emulsion and an oil-in-water (o/w) emulsion. 43.The method of claim 36, further comprising the step of adding anadditive.
 44. The method of claim 36, wherein the oil is selected fromthe group consisting of jojoba oil, rosehip oil, glycerin, coconut oil,lemongrass oil, shea butter, or a combination thereof.
 45. A method ofimproving skin hydration comprising applying a moisturizing compositiononce daily to human skin for a period of at least one week, wherein themoisturizing composition comprises: about 0.1% to about 5% silksolution, wherein the silk solution comprises about 1% to about 10%(w/v) of pure silk fibroin-based protein fragments that aresubstantially devoid of sericin; about 0.1% to about 5% (w/v) ofhyaluronic acid; about 0.1% to about 25% (v/v) of an oil or butter; andabout 0.1% to about 1.5% (v/v) of a pH adjusting agent.
 46. A method ofimproving skin hydration comprising applying a moisturizing compositiononce daily to human skin for a period of at least one week, wherein themoisturizing composition comprises: about 0.06% to about 0.3% (w/v) puresilk fibroin-based protein fragments that are substantially devoid ofsericin; about 0.1% to about 5% (w/v) of hyaluronic acid; about 0.1% toabout 25% (v/v) of an oil or butter; and about 0.1% to about 1.5% (v/v)of a pH adjusting agent.
 47. A method of improving skin hydrationcomprising applying a moisturizing composition once daily to human skinfor a period of at least one week, wherein the moisturizing compositioncomprises: about 1% to about 5% silk solution (v/v), wherein the silksolution comprises about 1% to about 10% (w/v) of pure silkfibroin-based protein fragments that are substantially devoid ofsericin; about 1% to about 3% (w/v) of hyaluronic acid; about 1% toabout 15% (v/v) of an oil or butter; and about 0.1% to about 1% (v/v) ofa pH adjusting agent.